High-Spin (meso-Tetraalkylporphyrinato)iron(III) Complexes As Studied by X-ray Crystallography, EPR, and Dynamic NMR Spectroscopies
Takahisa Ikeue; Yoshiki Ohgo; Akira Uchida; Mikio Nakamura; Hiroshi Fujii; Masataka Yokoyama; Inorganic Chemistry 38 (1999) 1276–1281; doi:10.1021/ic981184+

data_4327661
_publ_contact_author_address
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Department of Chemistry
Toho University 
5-21-16 Omorinishi Ota-ku TOKYO 143 JAPAN
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_publ_contact_author_email       mnakamu@med.toho-u.ac.jp
_publ_contact_author_fax         '81 3 5493 5430'
_publ_contact_author_name        'Nakamura, Mikio'
_publ_contact_author_phone       '81 3 3762 4151 x2551'
_publ_section_title
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 High-Spin (meso-Tetraalkylporphyrinato)iron(III) Complexes As Studied by
 X-ray Crystallography, EPR, and Dynamic NMR Spectroscopies
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1276
_journal_page_last               1281
_journal_paper_doi               10.1021/ic981184+
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H38 Cl Fe N4'
_chemical_formula_weight         521.92
_chemical_name_common            porphyrin
_chemical_name_systematic
; 
 ? 
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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.514(5)
_cell_length_b                   9.666(6)
_cell_length_c                   16.368(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      27.50
_cell_volume                     2771(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'RIGAKU AFC5'
_diffrn_measurement_method       W-2thetha
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3167
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        -0.559
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968).
Acta Cryst. A24, 351-359.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.093
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    calculated
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_obs          0.0470
_refine_ls_shift/esd_max         -0.040
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.5782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1397
_refine_ls_wR_factor_obs         0.1239
_reflns_number_observed          2419
_reflns_number_total             3167
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            ic9811842B.cif
_cod_data_source_block           (TiPrP)FeCl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.5782P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.5782P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2770.9(20)
_cod_database_code               4327661