Macromolecules 1c and 2c bearing multiple redox-active sites are synthesized by an efficient palladium-catalyzed coupling of 2, 5-dimethoxytolylmagnesium bromide with readily available hexakis (4-bromophenyl) benzene and tetrakis (4-bromophenyl) methane. These macromolecular electron donors undergo reversible oxidation at a constant potential of 1.15 V vs SCE to yield robust, multiply charged cation radicals that are isolated in pure form ...