Molecular Structures of Five-Coordinated Halide Ligated Iron(III) Porphyrin, Porphycene, and Corrphycene Complexes
Yoshiki Ohgo; Saburo Neya; Takahisa Ikeue; Masashi Takahashi; Masuo Takeda; Noriaki Funasaki; Mikio Nakamura; Inorganic Chemistry 41 (2002) 4627–4629; doi:10.1021/ic0256866

data_4318482
_publ_contact_author_address
;
Department of Chemistry
Toho University 
5-21-16 Omorinishi Ota-ku Tokyo 143 Japan
;
_publ_contact_author_email       yohgo@med.toho-u.ac.jp
_publ_contact_author_fax         '81 3 5493 5430'
_publ_contact_author_name        'Ohgo, Yoshiki'
_publ_contact_author_phone       '81 3 3762 4151 x2551'
_publ_section_title
;
 Molecular Structures of Five-Coordinated Halide Ligated Iron(III)
 Porphyrin, Porphycene, and Corrphycene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4627
_journal_page_last               4629
_journal_paper_doi               10.1021/ic0256866
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C33 H37 Br Cl3 Fe N4'
_chemical_formula_weight         731.78
_chemical_name_common            corrphycene
_chemical_name_systematic
; 
Bromo[(2,7,12,17-tetraethyl-3,6,11,18-
tetramethylcorrphycenato)iron(III)]
;
_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                84.862(6)
_cell_angle_beta                 89.610(8)
_cell_angle_gamma                74.100(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1544(9)
_cell_length_b                   12.2744(9)
_cell_length_c                   12.5930(13)
_cell_measurement_reflns_used    15222
_cell_measurement_temperature    298
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      3.2
_cell_volume                     1651.2(2)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software 
(Molecular Structure Corporation, 1992a)
;
_computing_data_reduction
;
MSC/AFC Diffractometer Control Software. Data Reduction: 
TEXSAN (Molecular Structure Corporation, 1992b)
;
_computing_molecular_graphics    'SV (Nemoto & Ohashi, 1993)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97(Altomare, A. et al., 1999)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'RIGAKU RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10430
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
ABSCOR(Higashi et al., 1968)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.253
_refine_ls_extinction_coef       0.076(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1174P)^2^+1.6619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2138
_reflns_number_gt                5362
_reflns_number_total             7121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0256866_s1_01.cif
_cod_data_source_block           '[Fe(EtioCn)Br]'
_cod_database_code               4318482