Electrocrystallization of C 6 0 in chlorobenzene and lithium tetraphenylborate in THF efficiently produced the new metallic species Li x C 6 0 (THF) y ; the ESR spectra show clearly the existence of a typical broad signal due to the C 6 0 anion radical. The change of the intensity of the ESR signal corresponds to the metal-insulator transition at 150 K, and the 1 3 C and 7 Li solid-state NMR spectra an also reported.