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_4318683
_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            'C24 H30 B2 F8 Fe N6 O'
_chemical_formula_weight         648.01
_chemical_name_common            '[(SBPy3)Fe(CH3CN)](BF4)2^.^0.33Et2O.0.67MeOH'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 103.422(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.398(15)
_cell_length_b                   11.859(5)
_cell_length_c                   12.783(5)
_cell_measurement_reflns_used    620
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.3
_cell_volume                     5662(4)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.067
_diffrn_reflns_av_sigmaI/netI    0.061
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37587
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            magenta
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+17.0513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1759
_reflns_number_gt                5681
_reflns_number_total             8565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic020373w_1.cif
_cod_data_source_block           mn1334
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4318683