We report the intercalation of ferrocene into Cd 2P 2S 6(CoCp 2) 0.8. The Cd 2P 2S 6 was first intercalated with cobaltocene, and then this intercalated material was reacted with ferrocene. Mass spectroscopy provides direct evidence for the presence of ferrocene in the Cd 2P 2S 6 host lattice. ESR measurements suggest that after the insertion of ferrocene into Cd 2P 2S 6(CoCp 2) 0.8, the concentration of neutral cobaltocene within Cd 2P 2S 6 is significantly reduced. X-ray diffraction and chemical analysis provide additional characterization.