Reversible (De)protonation-Induced Valence Inversion in Mixed-Valent Diiron(II,III) Complexes
Eric Gouré; Grégory Thiabaud; Michaël Carboni; Nathalie Gon; Patrick Dubourdeaux; Ricardo Garcia-Serres; Martin Clémancey; Jean-Louis Oddou; Adeline Y. Robin; Lilian Jacquamet; Lionel Dubois; Geneviève Blondin; Jean-Marc Latour; Inorganic Chemistry 50 (2011) 6408–6410; doi:10.1021/ic2007414

data_4325680
_publ_section_title
;
 Reversible (De)protonation-Induced Valence Inversion in Mixed-Valent
 Diiron(II,III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6408
_journal_page_last               6410
_journal_paper_doi               10.1021/ic2007414
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         {[Fe2(ON6C34H35)(O4C12H12)].2(ClO4).H2O}
_chemical_formula_sum            'C184 H196 Cl8 Fe8 N24 O56'
_chemical_formula_weight         4369.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   10.170(2)
_cell_length_b                   20.440(4)
_cell_length_c                   22.500(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4677.2(17)
_computing_cell_refinement       xds
_computing_data_collection       ADSC
_computing_data_reduction        xds
_computing_molecular_graphics    Schakal
_computing_publication_material  word
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.97959
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3120
_diffrn_reflns_theta_full        32.43
_diffrn_reflns_theta_max         32.43
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.810
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       'rhombohedral plates'
_exptl_crystal_F_000             2252
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+45.1776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                2860
_reflns_number_total             3120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2007414_si_002.cif
_cod_data_source_block           feaniline_test
_cod_original_cell_volume        4677.2(16)
_cod_database_code               4325680