Iron Tetraanthracenotetraazaporphyrins: Synthesis, Structural Characterization, Ligand Binding Properties, and Unexpected Selectivity of a Bis-"Bowl" Tetraazaporphyrin
Jeffrey P. Fitzgerald; Joshua R. Lebenson; Guangbin Wang; Gordon T. Yee; Bruce C. Noll; Roger D. Sommer; Inorganic Chemistry 47 (2008) 4520–4530; doi:10.1021/ic702149z

data_4304617
_publ_contact_author_address
;
United States Naval Academy
Annapolis, MD 21402
USA
;
_publ_contact_author_email       fitzgera@usna.edu
_publ_contact_author_fax         1(410)2932218
_publ_contact_author_name        'Jeffrey P. Fitzgerald'
_publ_contact_author_phone       1(410)2936343
_publ_section_title
;
Iron Tetraanthracenotetraazaporphyrins: Synthesis, Structural
Characterization, Ligand Binding Properties, and Unexpected Selectivity of
a Bis-"Bowl" Tetraazaporphyrin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4520
_journal_page_last               4530
_journal_paper_doi               10.1021/ic702149z
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C72 H40 N8 Cl Fe, 6(C H Cl3), 2(C6 H6)'
_chemical_formula_sum            'C90 H58 Cl19 Fe N8'
_chemical_formula_weight         1980.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_update_record
;
2007-10-30 # Formatted by publCIF
;
_cell_angle_alpha                104.785(1)
_cell_angle_beta                 110.180(1)
_cell_angle_gamma                102.081(1)
_cell_formula_units_Z            1
_cell_length_a                   13.0455(1)
_cell_length_b                   13.8818(1)
_cell_length_c                   14.8536(2)
_cell_measurement_reflns_used    6957
_cell_measurement_temperature    177(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.56
_cell_volume                     2306.46(5)
_computing_cell_refinement       'SAINT(Siemens 1995)'
_computing_data_collection       'SMART (Siemens 1995)'
_computing_data_reduction        'SAINT/XPREP(Siemens 1995)'
_computing_molecular_graphics    'XP(Siemens 1995)'
_computing_publication_material  'ENCIFER CCDC Ver 1.2'
_computing_structure_refinement  'XL (Siemens, 1997)'
_computing_structure_solution    'XS (Siemens 1995)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20420
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.9073
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (1995) University of G\"ottingen'
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1003
_exptl_crystal_recrystallization_method
'Slow evaporation of solvent from a chloroform/benzene/THF solution.'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
A large void, 1167 \%A^3^, exists in the structure. This void was occupied by 
electron density that could not be adequately modeled by conventional means.
The SQUEEZE routine of PLATON (Spek, 1997) was used to quantify the density 
present in this void. SQUEEZE found density equivalent to 426 electrons in 
this void space, which was taken as 6 molecules of chloroform and 2 of 
benzene, or 432 electrons. For the asymmetric unit, this yields a formula of
1/2^.^Fe(TATAP)Cl^.^C~6~H~6~^.^3CHCl~3~. Because SQUEEZE was used instead of 
an explicit model for the solvent molecules, quantities like molecular 
formula, formula weight, density, F(000), and \m will be miscalculated by 
routines such as checkCIF that generate this information from the atom list. 
The formula including solvent was used to calculate the data contained
herein.
;
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0933
_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^)+(0.1960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2587
_refine_ls_wR_factor_ref         0.2704
_reflns_number_gt                5893
_reflns_number_total             8098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702149z-file003.cif
_cod_data_source_block           bc249
_cod_original_cell_volume        2306.39(4)
_cod_database_code               4304617