Iron(III) and Iron(IV) Corroles: Synthesis, Spectroscopy, Structures, and No Indications for Corrole Radicals
Liliya Simkhovich; Israel Goldberg; Zeev Gross; Inorganic Chemistry 41 (2002) 5433–5439; doi:10.1021/ic020118b

data_4318664
_publ_section_title
;
 Iron(III) and Iron(IV) Corroles: Synthesis, Spectroscopy, Structures, and
 No Indications for Corrole Radicals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5433
_journal_page_last               5439
_journal_paper_doi               10.1021/ic020118b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '2(C47 H18 N6 F15 Fe).1.5(C7 H16)'
_chemical_formula_sum            'C104.5 H60 F30 Fe2 N12'
_chemical_formula_weight         2165.34
_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                101.3190(19)
_cell_angle_beta                 103.8850(17)
_cell_angle_gamma                93.244(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0800(5)
_cell_length_b                   16.6300(5)
_cell_length_c                   20.9740(8)
_cell_measurement_reflns_used    16319
_cell_measurement_temperature    115
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      1.85
_cell_volume                     4647.0(3)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      115
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 degree Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16319
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             2186
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         16319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.263
_refine_ls_shift/su_mean         0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+3.1296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1933
_reflns_number_gt                9766
_reflns_number_total             16319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020118b_1.cif
_cod_data_source_block           Fe(tpfc)(pyr)2
_cod_original_formula_sum        'C104.50 H60 F30 Fe2 N12'
_cod_database_code               4318664