The donors TTA and TSA were prepared starting from 1.5-dichloro-9.10-anthracenedione which was converted into 1.5.9.10-tetrachloroan-thracene (TCA) by two alternating chlorination and elimination steps. TCA was reacted under a dry argon atmosphere with suspensions of Na2S2and Na2Se2to yield TTA and TSA, respectively. Action of elemental iodine gives highly conductive polyiodides of both donors. Single crystals of TSA·I1.2actually behave metallic between 220 and 300 K. The X-ray structure of TSA and TSA·I1.2allows a comparison of intermolecular distances in the neutral and the partially oxidized, ionic stacks of the donor.