The new heterobimetallic [Mg(II)-Ti(IV)]-mu-oxoisopropoxide was synthesized on treatment of magnesium acetate with titanium(IV) isopropoxide in refluxing decalin in 1: 2 molar ratio and characterized by liberated isopropanol, elemental, spectral (IR, H-1 and C-13 NMR, and mass), thermal analysis, and molecular weight data. The reactions of [Mg(II)-Ti(IV)]-mu-oxoisopropoxide compound with beta-diketones in different molar ratios (1:1-1:4) yielded mono to tetra derivatives [{MgO2Ti2(OPri)(6-n)L-n}] (where n is 1-4 and L = acetylacetonate/benzoylacetonate anion)] of the mu-oxo complex and were characterized by elemental, liberated isopropanol, and spectral analysis (IR and H-1 and C-13 NMR). These studies revealed interesting facets in support of plausible structures of the parent compound and its beta-diketonates.