Unique Axial Imidazole Geometries of Fully Halogenated Iron(II) Porphyrin Complexes: Crystal Structures and Mössbauer Spectroscopic Studies.
Hu, Bin; He, Mingrui; Yao, Zhen; Schulz, Charles E.; Li, Jianfeng; Inorganic chemistry 55 (2016) 9632–9643; doi:10.1021/acs.inorgchem.6b01364

data_4348562
_publ_section_title
;
 Unique Axial Imidazole Geometries of Fully Halogenated Iron(II) Porphyrin
 Complexes: Crystal Structures and M\"ossbauer Spectroscopic Studies.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9632
_journal_page_last               9643
_journal_paper_doi               10.1021/acs.inorgchem.6b01364
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C52 H12 Br8 F20 Fe N8'
_chemical_formula_sum            'C52 H12 Br8 F20 Fe N8'
_chemical_formula_weight         1823.83
_chemical_name_common            '[Fe(TFPPBr8)(1-MeIm)2]'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                115.772(5)
_cell_angle_beta                 106.420(3)
_cell_angle_gamma                90.825(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4655(4)
_cell_length_b                   14.5702(6)
_cell_length_c                   15.1292(8)
_cell_measurement_reflns_used    4760
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9745
_cell_measurement_theta_min      2.9679
_cell_volume                     2719.4(2)
_computing_cell_refinement       'CrysAlisPro, Agilent,Version 1.171.35.19'
_computing_data_collection       'CrysAlisPro, Agilent,Version 1.171.35.19'
_computing_data_reduction        'CrysAlisPro, Agilent,Version 1.171.35.19'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 2008)'
_computing_publication_material  'XCIF (Sheldrick, 2008)/enCIFer (CCDC, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2141
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w 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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16978
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    6.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         9549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0342P)^2^+3.0511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                7230
_reflns_number_total             9549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01364_si_004.cif
_cod_data_source_block           fetfppbr_1_meim2_20140117
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4348562