A Four-Coordinate Fe(III) Porphyrin Cation
Ming Fang; Scott R. Wilson; Kenneth S. Suslick; Journal of the American Chemical Society 130 (2008) 1134–1135; doi:10.1021/ja078061l

data_4107360
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 A Four-Coordinate Fe(III) Porphyrin Cation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1134
_journal_page_last               1135
_journal_paper_doi               10.1021/ja078061l
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety
; 
C116 H188 Fe N4 O8 Si8, 0.6894(C H6 B11 Br6), 0.3106(C2 H12 B22 Br12 Ag), 
0.5(C H2 Cl2), C7 H16 
;
_chemical_formula_sum
'C998.48 H1702.91 Ag2.48 B115.33 Br62.91 Cl8 Fe8 N32 O64 Si64'
_chemical_formula_weight         24248.19
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2007-09-05   text and data added, mf 
@007-10-17   text and data added, mf 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   37.028(2)
_cell_length_b                   29.3262(19)
_cell_length_c                   29.3677(18)
_cell_measurement_reflns_used    4668
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      17.50
_cell_measurement_theta_min      2.50
_cell_volume                     31890(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction        'SAINT V7.23A (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga92tta
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_sigmaI/netI    0.5017
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            65276
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    2.226
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.5429
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       platy
_exptl_crystal_F_000             12564
_exptl_crystal_id                ga92tta
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.4 mm cryo-loop (Hampton Research) with the (-2 -1 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack (1983), 11,900 Friedels'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1939
_refine_ls_number_reflns         27861
_refine_ls_number_restraints     4123
_refine_ls_restrained_S_all      1.284
_refine_ls_R_factor_all          0.3398
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2398
_refine_ls_wR_factor_ref         0.2824
_reflns_number_gt                6424
_reflns_number_total             27861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja078061l-file005.cif
_cod_data_source_block           ga92ttapanis
_cod_original_sg_symbol_Hall     'C 2c -2 '
_cod_original_sg_symbol_H-M      'C m c 21 '
_cod_database_code               4107360