Complex [FeIIGdIII{pyCO(OEt)pyCOH(OEt)py}3](ClO4)2 (1) crystallizes in the Cc space group and contains one hexacoordinate ferrous ion and one enneacoordinate GdIII ion. Complex [Fe2IIGdIII{pyCO(OEt)py}4(NO3)(H2O)][Gd(NO3)5]0.5(ClO4) (2) crystallizes in the C2/c space group and contains two hexacoordinate ferrous ions and one octacoordinate GdIII ion. Both complexes have been prepared by the metal-assisted ethanolysis of ligands di-2,6-(2-pyridylcarbonyl)pyridine (pyCOpyCOpy, dpcp) and di-2-pyridyl ketone ((py)2CO, dpk), which exhibit similar structures. Mössbauer spectroscopic studies of 2 revealed the presence of two quadrupole-split doublets of equal intensities, each assigned to a ferrous site. These doublets exhibit similar isomer shifts (δ1 = 1.14 mm s−1, δ2 = 1.11 mm s−1) but quite different quadrupole splittings (ΔEQ1 = 3.55 mm s−1, ΔEQ2 = 2.74 mm s−1). Magnetic studies revealed weak ferromagnetic FeII–GdIII interactions for both complexes (JFeGd = +0.68 cm−1, DFe = 12.0 cm−1 for 1 and JFeGd = +0.03 cm−1, JFeFe = −1.73 cm−1 for 2, according to the -JSiSj spin-Hamiltonian formalism).
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