Synthesis, Characterization, and Autoreduction of a Highly Electron-Deficient Porphycenatoiron(III) with Trifluoromethyl Substituents
Takashi Hayashi; Yuji Nakashima; Kazuyuki Ito; Takahiro Ikegami; Isao Aritome; Katsuhiro Aoyagi; Tsutomu Ando; Yoshio Hisaeda; Inorganic Chemistry 42 (2003) 7345–7347; doi:10.1021/ic034757d

data_4312502
_publ_contact_author_address
; Department of Chemistry and Biochemistry
 Graduate School of Engineering
 Kyushu University
 Hakozaki Higashi-ku
 Fukuoka 812-8581
 Japan
;
_publ_contact_author_email       thayatcm@mbox.nc.kyushu-u.ac.jp
_publ_contact_author_fax         81(92)6423595
_publ_contact_author_name        'Prof. Takashi Hayashi'
_publ_contact_author_phone       81(92)6423595
_publ_section_title
;
 Synthesis, Characterization, and Autoreduction of a Highly
 Electron-Deficient Porphycenatoiron(III) with Trifluoromethyl
 Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7345
_journal_page_last               7347
_journal_paper_doi               10.1021/ic034757d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C65 H49 Cl3 F24 Fe2 N8 O'
_chemical_formula_sum            'C65 H49 Cl3 F24 Fe2 N8 O'
_chemical_formula_weight         1632.17
_chemical_name_systematic
; 
 \m-oxobis{[2,7,12,17-tetraethyl-3,6,13,16-
tetrakis(trifluoromethyl)porphycenato]iron} 
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5680(12)
_cell_length_b                   21.6097(19)
_cell_length_c                   21.0226(18)
_cell_measurement_reflns_used    4416
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.70
_cell_volume                     6618.1(10)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20487
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  758
_diffrn_standards_number         258
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_correction_T_min  0.8877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         5619
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                5012
_reflns_number_total             5619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034757dsi20030703_094717.cif
_cod_data_source_block           aba2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312502