<p> The products of the reaction between oxomethoxodichlorobistriphenylphosphinerhenium(V) and acetylacetone are determined, characterized and correlated in terms of a reaction scheme. A series of rhenium(III) compounds, characteristic of reactions analogous to the one mentioned above, with other β-ketoenols is prepared and characterized. The syntheses and properties of tris-1,1,1-5,5,5-hexafluoropentane-2,4-dionatorhenium(III) and trispentane-2,4-dionatorhenium(III) are described. A new nitrido-rhenium complex, nitridochloro-1,1,1-5,5,5-hexafluoropentane-2,4-dionatobistriphenylphosphinerhenium(V) complex is prepared and characterized. A synthetic route to pyridine-acetylacetonate complexes of rhenium is described. </p> / Thesis / Doctor of Philosophy (PhD)