Metalloporphyrin Mixed-Valence π-Cation Radicals: [Fe(oxoOEC./2)(Cl)]2SbCl6, Structure, Magnetic Properties, and Near-IR Spectra
Ming Li; Teresa J. Neal; Graeme R. A. Wyllie; Allen G. Oliver; Charles E. Schulz; W. Robert Scheidt; Inorganic Chemistry 50 (2011) 9114–9121; doi:10.1021/ic201292t

data_4326287
_publ_section_title
;
 Metalloporphyrin Mixed-Valence \p-Cation Radicals:
 [Fe(oxoOEC./2)(Cl)]2SbCl6, Structure, Magnetic Properties, and Near-IR
 Spectra
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9114
_journal_page_last               9121
_journal_paper_doi               10.1021/ic201292t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C37 H46 Cl6 Fe N4 O Sb0.5'
_chemical_formula_weight         892.20
_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                83.64(3)
_cell_angle_beta                 77.53(3)
_cell_angle_gamma                87.19(3)
_cell_formula_units_Z            2
_cell_length_a                   10.333(2)
_cell_length_b                   12.555(3)
_cell_length_c                   15.849(3)
_cell_measurement_reflns_used    226
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      14.5
_cell_volume                     1994.6(8)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      127(2)
_diffrn_detector_area_resol_mean 9.23
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Enraf-Nonius FAST area detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_av_sigmaI/netI    0.1155
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14683
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.3477
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       'flat plate'
_exptl_crystal_F_000             915
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1633
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1418P)^2^+7.9549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2397
_refine_ls_wR_factor_ref         0.2935
_reflns_number_gt                4166
_reflns_number_total             7319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201292t_si_002.cif
_cod_data_source_block           rev1
_cod_original_cell_volume        1994.6(7)
_cod_original_formula_sum        'C37 H46 Cl6 Fe N4 O Sb0.50'
_cod_database_code               4326287