Effect of Electron-Withdrawing Dithiolate Bridge on the Electron-Transfer Steps in Diiron Molecules Related to [2Fe]H Subsite of the [FeFe]-Hydrogenases
Kévin Charreteur; Mohamed Kdider; Jean-François Capon; Frédéric Gloaguen; François Y. Pétillon; Philippe Schollhammer; Jean Talarmin; Inorganic Chemistry 49 (2010) 2496–2501; doi:10.1021/ic902401k

data_4315083
_publ_contact_author_address
;Laboratoire de chimie,
electrochimie moleculaire et chimie analytique (UMR 6521)
Universite de Bretagne occidentale
6, avenue Victor Le Gorgeu
CS 93837
F-29238 BREST cedex 3
FRANCE 
;
_publ_contact_author_email       philippe.schollhammer@univ-brest.fr
_publ_contact_author_name        'Schollhammer, Philippe'
_publ_section_title
;
 Effect of Electron-Withdrawing Dithiolate Bridge on the Electron-Transfer
 Steps in Diiron Molecules Related to [2Fe]H Subsite of the
 [FeFe]-Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2496
_journal_page_last               2501
_journal_paper_doi               10.1021/ic902401k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
;
        2(C18 H4 Cl4 Fe2 O6 S2), C H2 Cl2
;
_chemical_formula_sum            'C37 H10 Cl10 Fe4 O12 S4'
_chemical_formula_weight         1352.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-11-17T20:34:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.900(2)
_cell_length_b                   12.0018(14)
_cell_length_c                   18.086(2)
_cell_measurement_reflns_used    2181
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      20.79
_cell_measurement_theta_min      2.75
_cell_volume                     4753.7(9)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method
;
4 stepped omega-scans over 115 deg. with kappa -79 deg. (chi -58.3 deg.),
        phi 0, 90, 180, 270 deg.
        step 1 deg., exposure time 240 s
        detector distance 50 mm
        detector angle 30 deg.
;
_diffrn_orient_matrix_UB_11      0.0309786872
_diffrn_orient_matrix_UB_12      0.0001812849
_diffrn_orient_matrix_UB_13      -0.0124127039
_diffrn_orient_matrix_UB_21      -0.0097504995
_diffrn_orient_matrix_UB_22      0.0167053773
_diffrn_orient_matrix_UB_23      -0.0359875983
_diffrn_orient_matrix_UB_31      0.0028557251
_diffrn_orient_matrix_UB_32      0.0571620848
_diffrn_orient_matrix_UB_33      0.0104031631
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2128
_diffrn_reflns_av_unetI/netI     0.1756
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30063
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
        (compiled Aug 27 2009,17:19:36)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.89
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
        fragment of flat rectangular needle,
        main faces {0 0 1}, long axis [0 1 0}
;
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                1995
_reflns_number_total             4052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902401k_si_002_2.cif
_cod_data_source_block           kc113-a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315083