We have investigated the charge transfer characteristics and electronic structure of ferrocene-intercalated TiSe2. The spectroscopic results revealed that an intercalation of metallocene molecules leads to changes in the ionic valence of Fe atom in ferrocene molecule and the band gap, which is in accordance with electrical resistivity measurements showing metallic conductivity. Our analysis of Fe-57 Mossbauer and Fe 2p XAS spectra suggested that the suppression of charge-density-wave state in TiSe2 and an appearance of metallic conductivity are attributed to charge transfer of electrons from ferrocene intercalant to the dichalcogenide host material. (c) 2010 Published by Elsevier B.V.