Oxidatively Induced Reactivity of [Fe2(CO)4(κ2-dppe)(μ-pdt)]: an Electrochemical and Theoretical Study of the Structure Change and Ligand Binding Processes
Dounia Chouffai; Giuseppe Zampella; Jean-François Capon; Luca De Gioia; Frédéric Gloaguen; François Y. Pétillon; Philippe Schollhammer; Jean Talarmin; Inorganic Chemistry 50 (2011) 12575–12585; doi:10.1021/ic201601q

data_4327112
_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
;
 Oxidatively Induced Reactivity of [Fe2(CO)4(\k2-dppe)(\m-pdt)]: an
 Electrochemical and Theoretical Study of the Structure Change and Ligand
 Binding Processes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12575
_journal_page_last               12585
_journal_paper_doi               10.1021/ic201601q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
;
        C35 H39 Fe2 O6 P3 S2, C H2 Cl2, C6 H14
;
_chemical_formula_sum            'C42 H55 Cl2 Fe2 O6 P3 S2'
_chemical_formula_weight         995.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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             2009-04-20T18:56:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.334(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9360(9)
_cell_length_b                   10.7232(5)
_cell_length_c                   25.4174(13)
_cell_measurement_reflns_used    5476
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.31
_cell_volume                     4608.2(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR2'
_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 150 s
        detector distance 50 mm
        detector angle 30 deg.
;
_diffrn_orient_matrix_UB_11      -0.0014441551
_diffrn_orient_matrix_UB_12      -0.0091014049
_diffrn_orient_matrix_UB_13      0.027572945
_diffrn_orient_matrix_UB_21      0.0409811846
_diffrn_orient_matrix_UB_22      0.0134722953
_diffrn_orient_matrix_UB_23      0.0033362505
_diffrn_orient_matrix_UB_31      -0.0088600723
_diffrn_orient_matrix_UB_32      0.0640986347
_diffrn_orient_matrix_UB_33      0.0032238135
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.1324
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31636
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.8
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description
;
        flat prism, main axis [0 1 0], main faces {1 0 1}, {0 0 1}
;
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1829
_reflns_number_gt                4941
_reflns_number_total             8405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201601q_si_002.cif
_cod_data_source_block           dc2-b0
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4327112