Superconducting radical cation salts derived from the donor molecule bis(ethylenedithio)tetrathiafulvalene (ET) are an important class of molecular organic conductors. Superconducting ET-iodine phases, owing to relatively high transition temperatures, are playing a key role in the development of prototypic devices. Here is reported a novel redox preparation of the organic metal alpha-(ET)(2)I-3, as well as a study of the thermally induced conversion of this material and the structural characterization and superconducting properties of the transformation product.