Characterization of the "Absent" Vanadium Oxo V(═O){N(SiMe3 )2 }3 , Imido V(═NSiMe3 ){N(SiMe3 )2 }3 , and Imido-Siloxy V(═NSiMe3 )(OSiMe3 ){N(SiMe3 )2 }2 Complexes Derived from V{N(SiMe3 )2 }3 and Kinetic Study of the Spontaneous Conversion of the Oxo Complex into Its Imido-Siloxy Isomer

Inorganic Chemistry
Cary R StennettPhilip P Power

Abstract

The synthesis and characterization of V(═O){N(SiMe3)2}3 (1), V(═NSiMe3){N(SiMe3)2}3 (2), and V(═NSiMe3)(OSiMe3){N(SiMe3)2}2 (3) are described. Prior attempts to synthesize the vanadium(V) oxo complex 1 via salt metathesis of VOCl3 with the lithium or sodium silylamide salt had yielded either the putative rearranged species V(═NSiMe3)(OSiMe3){N(SiMe3)2}2 (3) or the oxo-bridged, dimetallic {(μ-O)2V2[N(SiMe3)2]4}. We now show that complex 1 is available by treatment of the vanadium(III) tris(silylamide) V{N(SiMe3)2}3 with iodosylbenzene. The imido complex 2 was obtained by treatment of V{N(SiMe3)2}3 with trimethylsilyl azide. Sublimation of 1 formed complex 3, which was determined to be V(═NSiMe3)(OSiMe3){N(SiMe3)2}2, on the basis of infrared, electronic, and 1H and 51V NMR spectroscopies. Crystallographic disorder precluded a complete structural characterization of 3, although a four-coordinate V atom, as well as severely disordered ligands, were apparent. Comparison of the vibrational spectra of 1 and 2 allowed an unambiguous assignment of the V-O (995 cm-1) and V-Nimide (1060 cm-1) stretching bands. The vibrational spectrum of complex 3 displayed strong absorbances at 1090 and 945 cm-1, indicative of its metal imide and metal s...Continue Reading

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