The long-lived ethylene, cyclohexene, and norbornenemercurinium ions prepared in superacidic, low-nucleophilic media have been studied by (13)C and (199)Hg NMR spectroscopy. The norbornenemercurinium ion shows temperature-dependent (13)C and (199)Hg NMR spectra, consistent with equilibration via rapid hydride and Wagner-Meerwin shifts. The (199)Hg NMR shifts of a series of alkylmercury bromides were also obtained in order to elucidate the effect of methyl substituents on (199)Hg NMR chemical shifts.