Synthesis and characterization of chlorobis(cyclopentadienyl) titanium(IV) and zirconium(IV) O,O'-dialkyl and alkylene dithiophosphates

摘要

Reactions of O,O'-dialkyl and alkylene dithiophosphoric acids with bis (cyclopentadienyl) titanium(IV) and zirconium (IV) dichloride in a 1:1 molar ratio in refluxing benzene proceeds with elimination of HCl and formation of the substituted derivatives, Cp _2MCl[S _2P(OR) _2] (where R = Et, Pr-n, Pr-i, Bu-i and Ph), Cp _2MCl[S _2POGO] (where G = -CH _2CMe _2CH _2-, -CH _2CEt_2CH _2- and -CMe _2CMe _2-), (M = Ti and Zr). The complexes are dark red and yellow solids, soluble in common organic solvents and monomeric in nature. These have been characterized on the basis of elemental analyses, molecular weight determinations, IR, and NMR (~1H, ~(13)C, and ~(31)P).