A five-coordinate iron(III) porphyrin complex including a neutral axial pyridine <i>N</i>-oxide ligand
Short, Melanie A.; Sommer, Roger D.; Falzone, Alec J.; Huang, Tao; Weare, Walter W.; Roizen, Jennifer L.; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619005849

data_2021634
_publ_section_title
;
 A five-coordinate iron(III) porphyrin complex including a neutral axial
 pyridine <i>N</i>-oxide ligand
;
_journal_coeditor_code           FN3305
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619005849
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Fe (C44 H28 N4) (C5 H5 N O)] [Sb F6], 2C H2 Cl2'
_chemical_formula_moiety         'C49 H33 Fe N5 O +, F6 Sb -, 2(C H2 Cl2)'
_chemical_formula_sum            'C51 H37 Cl4 F6 Fe N5 O Sb'
_chemical_formula_weight         1169.25
_chemical_name_common            '[Fe(TPP)pyrNO]SbF6'
_chemical_name_systematic
;(Pyridine <i>N</i>-oxide-\k<i>O</i>)(5,10,15,20-tetraphenylporphinato-\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')iron(III)
hexafluoroantimonate(V) dichloromethane disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                97.8276(13)
_cell_angle_beta                 105.1730(13)
_cell_angle_gamma                90.3499(13)
_cell_formula_units_Z            4
_cell_length_a                   15.3886(4)
_cell_length_b                   15.9246(4)
_cell_length_c                   20.2111(5)
_cell_measurement_reflns_used    599
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      29.9433
_cell_measurement_theta_min      2.4090
_cell_volume                     4731.2(2)
_computing_cell_refinement
;
APEX3 (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker--Nonius X8 Kappa APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            245803
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         1.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.714
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1352
_refine_ls_number_reflns         32919
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+5.1106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                25859
_reflns_number_total             32919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3305sup1.cif
_cod_data_source_block           I
_cod_database_code               2021634
_shelx_hkl_checksum              87667
_shelx_res_checksum              82696
_cod_database_fobs_code 2021634