[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_4113208
_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         'C15 H22 Fe2 N6 O S2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C17 H25 F12 Fe2 N7 O P2 S2'
_chemical_formula_weight         809.20
_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
; 
2003-08-22   text and data added, cad 
;
_cell_angle_alpha                115.826(7)
_cell_angle_beta                 108.787(7)
_cell_angle_gamma                96.105(8)
_cell_formula_units_Z            2
_cell_length_a                   11.761(5)
_cell_length_b                   12.343(6)
_cell_length_c                   13.096(6)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.53
_cell_volume                     1550.7(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  p44ua
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16080
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  433
_diffrn_standards_number         81
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_correction_T_min  0.7362
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       prism
_exptl_crystal_F_000             812
_exptl_crystal_id                p44ua
_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 -1 -1) scattering planes roughly 
normal to the spindle axis. 
;
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     1710
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                3725
_reflns_number_total             5679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049050ksi20040219_042706.cif
_cod_data_source_block           p44ua
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113208