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_4318666
_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         '(C37 H17 N4 Cl6 Fe).NO.2(C6 H6)'
_chemical_formula_sum            'C49 H29 Cl6 Fe N5 O'
_chemical_formula_weight         972.32
_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                 100.8890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.6430(13)
_cell_length_b                   14.5000(3)
_cell_length_c                   15.8420(5)
_cell_measurement_reflns_used    7696
_cell_measurement_temperature    115
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.06
_cell_volume                     8716.8(4)
_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 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. 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    0.0565
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7696
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.199
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+41.2281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                5630
_reflns_number_total             7696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020118b_3.cif
_cod_data_source_block           Fe(tdcc)(NO)
_cod_database_code               4318666