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Date of Award
Charles H. Winter
Treatment of tetrakis(dimethylamido)zirconium with four equivalents of primary and secondary amides in refluxing toluene, followed by sublimation of the crude products afforded tetrakis(N-tert-butylacetamido)zirconium, tetrakis(N-isopropylisobutyramido)zirconium, tetrakis(N-isopropylacetamido)-zirconium, tetrakis(N-methylacetamido)zirconium, and tetrakis(N-tert-butylformamido)zirconium as colorless crystalline solids. The structural assignments for the new complexes were based upon spectral and analytical data and by X-ray crystal structure determinations for tetrakis(N-tert-butylacetamido)zirconium, tetrakis(N-isopropylacetamido)zirconium, tetrakis(N-methylacetamido)zirconium, and tetrakis(N-tert-butylformamido)zirconium. These complexes are monomeric in the solid state, with eight-coordinate metal centers surrounded by four k2-amidate ligands. Solid state decomposition temperatures for the zirconium complexes range between 218-335 degrees Celsius.
Treatment of tris(tert-butylperoxy)borane with one equivalent of 4-dimethylaminopyridine or ammonia, quantitatively yielded colorless crystalline complexes. The structural assignment for the 4-dimethylaminopyridine adduct was based upon spectral and X-ray crystal structure determinations.
The thermal stability and volatility evaluation of bis[tris(pyrazolyl)borate]ruthenium(II) is reported as a potential precursor for the deposition of ruthenium containing films.
Baumann, Joseph William, "Synthesis And Characterization Of Boron And Zirconium Complexes" (2018). Wayne State University Theses. 610.