The synthesis of l, 4-[(RCp), Ti], Sep (R= H (3a), Me (3b), i-Pr (3c) is described together with their applications to the preparation of 1, 2, 5, 6-Se4S4 (4). The deselenization of (RCp), TiSe5 (2a-c) with organophosphines gives 3a-c isolated as purple microcrystalline solids. The same compounds could also be prepared from the reaction of (RCp), TiCI, with solutions of Li2Se2. RCp labeling studies show that these Ti2Se4 compounds do not ...