Synthesis and Characterization of Oxo- and Dihalovanadium(IV) and Oxovanadium(V) Imine/Phenolate Complexes
Webb, Kathleen K.
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The occurrence of vanadium in nature has been explored extensively in the last twenty years. However, in many cases its specific role in different environments is not completely understood. Therefore an exploration of the coordination and reactivity of vanadium complexes has been started. This has led to interest in the reactivity of oxo- and dihalovanadium(IV) and oxovanadium(V) compounds. In this project several imine/phenolate systems were both synthsized and characterized. Literature results were reproduced, and some interesting features were found. The characteristic stretch in the infrared spectrum for the vanadyl (V=02+) group was observed at different frequencies depending on the nature of the complex and the coordination environment. Most of the vanadium(IV) complexes showed a characteristic stretch in the 950-lOOOcnr1 region, with the exception of two whose solid state structure is in a polymeric form. And the primary evidence that the dihalovanadium reaction proceeds, is the disappearance of the vanadyl peak in the infrared spectrum. The vanadium(V) complexes show the incorporation of the tetrafluoroborate anion, and a shift in the observed v(V=0). The preparation of these vanadium(V) complexes with NOBF4 was refined with respect to previous use. Complexes were isolated with ease, and some in crystalline form. These complexes were structurally characterized using infrared, electronic, and nuclear magnetic spectroscopy where possible.