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_4318489
_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            'C32 H36 Br Fe N4'
_chemical_formula_weight         612.41
_chemical_name_common            porphyrin
_chemical_name_systematic
; 
Bromo[2,7,12,17-tetraethyl-3,8,13,18-
tetramethylporphyrinato]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                91.191(7)
_cell_angle_beta                 92.289(3)
_cell_angle_gamma                98.406(8)
_cell_formula_units_Z            4
_cell_length_a                   10.3871(7)
_cell_length_b                   14.6242(15)
_cell_length_c                   18.8842(8)
_cell_measurement_reflns_used    16250
_cell_measurement_temperature    298
_cell_measurement_theta_max      50.7
_cell_measurement_theta_min      2.8
_cell_volume                     2834.5(4)
_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 0.796
_diffrn_measured_fraction_theta_max 0.796
_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  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10216
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
ABSCOR(Higashi et al., 1968)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0104(18)
_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   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         9897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0944
_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^)+(0.1938P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2684
_reflns_number_gt                7423
_reflns_number_total             9897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0256866_s1_08.cif
_cod_data_source_block           '[Fe(EtioP)Br]'
_cod_database_code               4318489