A new bis-α-hydrogen nitroxide based initiator for use in nitroxide-mediated free radical polymerization (NMRP) has been synthesized and is demonstrated to effect controlled polymerizations. The bisnitroxide forms “living” systems; the resulting polymers are formed with low polydispersities. The addition of a second block is facile, forming symmetrical ABA triblock copolymers. Monomer addition occurs at the center of the living polymer. This “ ...