NMR and EPR Spectroscopic and Structural Studies of Low-Spin, (dxz,dyz)4(dxy)1 Ground State Fe(III) Bis-tert-Butylisocyanide Complexes of Dodecasubstituted Porphyrins
Liliya A. Yatsunyk; F. Ann Walker; Inorganic Chemistry 43 (2004) 4341–4352; doi:10.1021/ic035242p

data_4311216
_publ_contact_author_address
;
     University of Arizona
     Department of Chemistry
     1306 E. University
     Tucson, AZ 85721-0041
     USA
;
_publ_contact_author_email       liliya@u.arizona.edu
_publ_contact_author_fax         520-621-8407
_publ_contact_author_name        'Liliya Yatsunyk, Dr. Ann Walker'
_publ_contact_author_phone       520-621-9697
_publ_section_title
;
 NMR and EPR Spectroscopic and Structural Studies of Low-Spin,
 (dxz,dyz)4(dxy)1 Ground State Fe(III) Bis-tert-Butylisocyanide Complexes
 of Dodecasubstituted Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4341
_journal_page_last               4352
_journal_paper_doi               10.1021/ic035242p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_analytical     'Fe N6 C62 H62'
_chemical_formula_iupac
;
[Fe N6 C62 H62](Cl O4)*1(C H2 Cl2) 1.4(C12 H26)
;
_chemical_formula_moiety         'Fe N6 C62 H62 +, Cl O4 -, C H2 Cl2, C17 H35'
_chemical_formula_structural
;
[Fe (N4 C52 H44) (C5 H9 N)2]+ 1(Cl O4)- 1(C H2 Cl2) 1.4(C12 H26) 
;
_chemical_formula_sum            'C80 H99 Cl3 Fe N6 O4'
_chemical_formula_weight         1370.85
_chemical_name_common            '[Fe(III)OMTPP(t-BuNC)2]ClO4'
_chemical_name_systematic
; 
 bis{tert-butylisocyanide}octamethyltetraphenylporphyrinato 
Iron(III) perchloride 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   29.311(4)
_cell_length_b                   17.068(2)
_cell_length_c                   14.0209(19)
_cell_measurement_reflns_used    4221
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.773
_cell_measurement_theta_min      2.338
_cell_volume                     7014.4(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1344
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43978
_diffrn_reflns_theta_full        20.84
_diffrn_reflns_theta_max         20.84
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0.03
_diffrn_standards_interval_count 1818
_diffrn_standards_number         97
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.8738
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         3834
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0788P)^2^+30.0417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                2194
_reflns_number_total             3834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035242psi20031027_045555.cif
_cod_data_source_block           ly06a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:
'_symmetry_space_group_number' data item was removed -- it should
have been renamed to '_space_group_IT_number' as specified in the
replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst',
but the replacement data item was already present in the data block
and had the same value as the '_symmetry_space_group_number' data
item.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        7014.5(16)
_cod_original_sg_symbol_Hall     Pnma
_cod_database_code               4311216