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The radical anions and radical cations of two alkyl-substituted non-alternant hydrocarbons, 1,3,5,7-tetra-tert-butyl-s-indacene and 2,7-di-tert-butyldicyclopenta [a,e] cyclooctene, were characterized by their proton coupling constants with the use of ESR and, in part, ENDOR spectroscopy. Considering the unusual electronic structures of the π-systems in question, these values agree fairly well with those predicted by simple MO theory. Also reported are the proton hyperfine data for the radical ions of the likewise alkyl-substituted non-alternant 8,16-diisopropyl-s-indaceno [1,2,3-cd:5,6,7-c′ d′] diphenalene.