Structural, NMR, and EPR Studies of S=1/2 and S=3/2 Fe(III) Bis(4-Cyanopyridine) Complexes of Dodecasubstituted Porphyrins
Liliya A. Yatsunyk; F. Ann Walker; Inorganic Chemistry 43 (2004) 757–777; doi:10.1021/ic035010q

data_4310450
_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         520-621-9300
_publ_contact_author_name        'Liliya Yatsunyk'
_publ_contact_author_phone       520-621-9697
_publ_section_title
;
 Structural, NMR, and EPR Studies of S=1/2 and S=3/2 Fe(III)
 Bis(4-Cyanopyridine) Complexes of Dodecasubstituted Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              757
_journal_page_last               777
_journal_paper_doi               10.1021/ic035010q
_journal_volume                  43
_journal_year                    2004
_chemical_formula_analytical     'Fe N8 C64 H52'
_chemical_formula_iupac          '[Fe N8 C64 H52](Cl O4) * (C H Cl3)'
_chemical_formula_structural
; 
[Fe (N4 C52 H44) (N4 C12 H8)]+ (Cl O4)- (C H Cl3) 
;
_chemical_formula_sum            'C65 H53 Cl4 Fe N8 O4'
_chemical_formula_weight         1207.80
_chemical_name_common            '[FeOMTPP(4-CNPy)2]ClO4'
_chemical_name_systematic
; 
 bis{4-cyanopyridine}octamethyltetraphenylporphinato 
Iron(III) perchlorate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 98.505(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7529(16)
_cell_length_b                   23.115(3)
_cell_length_c                   17.3580(19)
_cell_measurement_reflns_used    6249
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      21.4345
_cell_measurement_theta_min      2.248
_cell_volume                     5854.2(12)
_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  'Brucker SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Brucker SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0925
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68928
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 1818
_diffrn_standards_number         79
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.8532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         12736
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0652P)^2^+2.9656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                7641
_reflns_number_total             12736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035010qsi20030827_074728.cif
_cod_data_source_block           sad2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        5854.2(11)
_cod_original_sg_symbol_Hall     P2(1)/n
_cod_database_code               4310450