Journal of Porphyrins and Phthalocyanines p. 254 - 264 (2016)
Update date:2022-09-26
Topics:
Serth-Guzzo, Judith A.
Turowska-Tyrk, Ilona
Safo, Martin K.
Walker, F. Ann
Debrunner, Peter G.
Robert Scheidt
The reaction of [Fe(TMP)(OClO3)], where TMP is the dianion of tetramesitylporphyrin, with a combination of a strong-acceptor ligand and a-donating imidazole can lead to the preparation of mixed-ligand complexes [Fe(Porph)(4-CNPy)(L)]+ where L is imidazole itself or 1-acetylimidazole and 4-cyanopyridine is the strong acceptor ligand. The stability of the new mixed-ligand pair is the presumed result of synergic bonding between the two axial ligands. The molecular structure and other characterization of the new mixed axial ligand complex, [Fe(TMP)(4-CNPy)(HIm)]ClO4 is described. The axial ligands have a relative perpendicular arrangement with Fe-N(imidazole) = 1.945 ? and Fe-N(pyridine) = 2.021 ?. The average equatorial Fe-Np distance is 1.963 ?, which is consistent with the S4-ruffled TMP core. Despite the relative perpendicular arrangement of axial ligands, the EPR spectrum of the complex is a rhombic signal and not a large gmax signal. The EPR g-values are g1 = 3.05, g2 = 2.07, and g3 = 1.22. A quadrupole doublet was seen in the M?ssbauer spectrum with an isomer shift of 0.197 mm/s and quadrupole splitting of 1.935 mm/s. Two crystalline forms of [Fe(TMP)(4-CNPy)(HIm)]ClO4 have been characterized; the two forms differ only in the solvent content of the lattice. Crystal data for form A: a = 15.432 (12) ?, b = 20.696 (2) ?, c = 19.970 (5) ?, and β = 99.256 (14)deg, monoclinic, space group P21/n, V = 6295 (2) ?3, Z = 4, formula FeCl3O4N8C69H69, 8397 observed data, R1 = 0.086, wR2 = 0.210, refinement on F2. Crystal data for form B: a =15.267 (3) ?, b =20.377 (6) ?, c = 19.670 (4) ?, and β = 98.14 (1)deg, monoclinic, space group P21/n, V = 6058 (4) ?3, Z = 4, formula C65.25H60.5Cl1.5FeN8O4, 5464 observed data, R1 = 0.096, wR2 = 0.112, refinement on F.
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