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The reaction of poly(hydromethylsiloxane-co-methylphenylsiloxane) with zirconium (IV) n-propoxide in dry toluene leads to extensive scission of the siloxane chain and conversion of Si-H groups. These processes produce oligomeric siloxanes and organosilanes containing moisture sensitive propoxy and siloxy-zirconate groups. The obtained post-reaction solution of zirconium containing heterosiloxane oligomers is stable under anhydrous conditions for several weeks. However, its exposure to moisture initiates the hydrolytic condensation of the