Electrochemical and theoretical investigations of the reduction of [Fe2(CO)5L{µ-SCH2XCH2S}] complexes related to [FeFe] hydrogenase
Capon, Jean-François; Ezzaher, Salah; Gloaguen, Frédéric; Pétillon, François Y.; Schollhammer, Philippe; Talarmin, Jean; Davin, Thomas J.; McGrady, John E.; Muir, Kenneth W.; New Journal of Chemistry 31 (2007) 2052–; doi:10.1039/b709273c

data_7052214
_publ_section_title
;
 Electrochemical and theoretical investigations of the reduction of
 [Fe2(CO)5L{&#x00B5;-SCH2XCH2S}] complexes related to [FeFe]
 hydrogenase
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2052
_journal_paper_doi               10.1039/b709273c
_journal_volume                  31
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C11 H11 Fe2 N1 O7 S2'
_chemical_formula_sum            'C11 H11 Fe2 N O7 S2'
_chemical_formula_weight         445.03
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2004-06-17T09:21:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                73.116(3)
_cell_angle_beta                 78.757(3)
_cell_angle_gamma                86.088(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4291(4)
_cell_length_b                   9.8933(6)
_cell_length_c                   11.8779(7)
_cell_measurement_reflns_used    23518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     819.28(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.135487
_diffrn_orient_matrix_UB_12      0.17555E-2
_diffrn_orient_matrix_UB_13      0.295422E-1
_diffrn_orient_matrix_UB_21      0.182665E-1
_diffrn_orient_matrix_UB_22      -0.56184E-1
_diffrn_orient_matrix_UB_23      0.818589E-1
_diffrn_orient_matrix_UB_31      0.121291E-1
_diffrn_orient_matrix_UB_32      0.894428E-1
_diffrn_orient_matrix_UB_33      0.209025E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12557
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.057
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.58
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                3911
_reflns_number_total             4735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709273c.txt
_cod_data_source_block           km1203
_cod_database_code               7052214