Alkyl thioglycolates of the type Al(OR)G (R = Pr i , Bu t ); M(OR) 2 G (M = Ti, Zr; R = Pr i , Bu t ); MG 2 (M = Ti, Zr), Al 2 G 3 and Al(GH)G where GH 2 is methyl or ethyl thioglycolate have been prepared. The isopropoxy derivatives were obtained by carrying out the reaction between the isopropoxide of the corresponding metal with methyl or ethyl thioglycolate in anhydrous benzene in different molar ratios, whereas the tertiary butoxy derivatives were prepared from the respective isopropoxy derivatives by alcohol interchange technique. Molecular weights of soluble titanium and zirconium derivatives show them to be dimeric in nature. Structures have been suggested on the basis of infrared spectral and molecular weight studies.