Synthesis and Crystal Structure Determination of Di-μ-Oxo Bis[oxovanadium(V)] Complexes Derived From 2-Ethoxy-6-[(2-methylaminoethylimino)methyl]phenol and 2-Methoxy-6-[(2-phenylaminoethylimino)methyl]phenol

Abstract

The reaction of vanadyl acetylacetonate with 2-ethoxy-6-[(2-methylaminoethylimino)methyl]phenol (EMP) and 2-methoxy-6-[(2-phenylaminoethylimino)methyl]phenol (MMP), respectively, affords two oxo-bridged dinuclear Schiff base vanadium(V) complexes, [VO2(EMP)]2 and [VO2(MMP)]2. The structures of the complexes were characterized by elemental analysis, infrared spectroscopy, and single-crystal X-ray diffraction. Complex [VO2(EMP)]2 crystallizes as monoclinic space group C2/c, with a = 24.342(2), b = 6.686(1), c = 17.206(1) Å, β = 103.980(2)°, V = 2717.3(5) Å3, Z = 4, R 1 = 0.0874, wR 2 = 0.2024 for 1781 observed data. Complex [VO2(MMP)]2 crystallizes as monoclinic space group P21/c, with a = 12.545(1), b = 17.641(2), c = 6.953(1) Å, β = 93.279(2)°, V = 1536.2(4) Å3, Z = 4, R 1 = 0.0907, wR 2 = 0.2229 for 2097 observed data. The complexes exhibit distorted octahedral geometry, involving in the equatorial plane the phenolate, imine, and amine donors of the Schiff base ligand and the bridging oxo O group and in the axial positions two other oxo O groups. The intramolecular V···V distances are 3.090(1) Å in [VO2(EMP)]2 and 3.096(1) Å in [VO2(MMP)]2.