Deprotonation in Mixed-Valent Diiron(II,III) Complexes with Aniline or Benzimidazole Ligands.
Gouré, Eric; Carboni, Michaël; Troussier, Angélique; Dubourdeaux, Patrick; Clémancey, Martin; Gon, Nathalie; Balasubramanian, Ramachandran; Lebrun, Colette; Pécaut, Jacques; Blondin, Geneviève; Latour, Jean-Marc; Inorganic chemistry 54 (2015) 6257–6266; doi:10.1021/acs.inorgchem.5b00449

data_4343380
_publ_section_title
;
 Deprotonation in Mixed-Valent Diiron(II,III) Complexes with Aniline or
 Benzimidazole Ligands.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6257
_journal_page_last               6266
_journal_paper_doi               10.1021/acs.inorgchem.5b00449
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C49 H47 Fe2 N8 O5, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C53 H53 Cl2 Fe2 N10 O13'
_chemical_formula_weight         1220.65
_chemical_name_common            '[Fe{L-(Py)2(BzImH)2}(mpdp)Fe](ClO4)2.2CH3CN'
_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
_cell_angle_alpha                74.765(5)
_cell_angle_beta                 71.367(6)
_cell_angle_gamma                71.904(5)
_cell_formula_units_Z            2
_cell_length_a                   12.3827(9)
_cell_length_b                   13.2351(7)
_cell_length_c                   18.8207(11)
_cell_measurement_reflns_used    6770
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4000
_cell_measurement_theta_min      3.3298
_cell_volume                     2732.0(3)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
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(compiled Oct 25 2010,18:11:34)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -5.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489   77.0000  120.0000 70

  2 omega    2.00   94.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489   77.0000 -150.0000 92

  3 omega  -41.00   97.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489    0.0000   30.0000 138

  4 omega  -45.00    1.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000 -120.0000 46

  5 omega  -71.00  -42.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000   90.0000 29

  6 omega    6.00   42.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000    0.0000 36

  7 omega  -56.00  -28.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000    0.0000 28

  8 omega -103.00  -44.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  179.0000  -90.0000 59

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28892
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.8013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         13554
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.3980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                9255
_reflns_number_total             13554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00449_si_002.cif
_cod_data_source_block           mc375
_cod_depositor_comments
'Adding full bibliography for 4343379--4343380.cif.'
_cod_database_code               4343380