Spontaneous Reduction of a Low-Spin Fe(III) Complex of a Neutral Pentadentate N5 Schiff Base Ligand to the Corresponding Fe(II) Species in Acetonitrile
Apurba K. Patra; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 41 (2002) 5403–5409; doi:10.1021/ic020373w

data_4318685
_publ_section_title
;
 Spontaneous Reduction of a Low-Spin Fe(III) Complex of a Neutral
 Pentadentate N5 Schiff Base Ligand to the Corresponding Fe(II) Species in
 Acetonitrile
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5403
_journal_page_last               5409
_journal_paper_doi               10.1021/ic020373w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C43.6 H50.8 Cl4 Fe2 N10 O19'
_chemical_formula_weight         1272.44
_chemical_name_common
'[(SBPy3)FeOFe(SBPy3)](ClO4)4^.^1.2acetone^.^0.8H2O'
_chemical_name_systematic
;
  ?
;
_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                94.408(15)
_cell_angle_beta                 95.638(17)
_cell_angle_gamma                115.82(2)
_cell_formula_units_Z            2
_cell_length_a                   12.543(5)
_cell_length_b                   13.258(6)
_cell_length_c                   19.381(8)
_cell_measurement_reflns_used    796
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     2861(2)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.090
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31042
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1309
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.776
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.0049(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         13035
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.102
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+15.3361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2402
_refine_ls_wR_factor_ref         0.2672
_reflns_number_gt                8510
_reflns_number_total             13035
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic020373w_3.cif
_cod_data_source_block           mn1356
_cod_original_formula_sum        'C43.60 H50.80 Cl4 Fe2 N10 O19'
_cod_database_code               4318685