Disilane unit containing polytitana- and polyzirconasiloxanes were synthesized by the reaction of 1,1,2,2-tetramethyl-1,2-disilanediol with bis(2,4-pentanedionato)titanium diisopropoxide or bis(2,4-pentanedionato)zirconium diisopropoxide. These polymers consisted of disilane unit and metalloxane bonding as main chain with pendants of methyl and 2,4-pentanedionato groups and terminals of isopropoxy and silanol groups. On the other hand, a cyclotitanasiloxane was prepared by the reaction of 1,1,2,2-tetramethyl-1,2-disilanedioI with titanocene dichloride in the presence of triethylamine.