Abstract The synthesis of di-t-butyl ditelluride, t-Bu 2 Te 2, and di-t-butyl telluride, t-Bu 2 Te, are reported together with that of di-(neo-hexyl) ditelluride. New syntheses of Me 2 Te 2 and i-Pr 2 Te 2 are presented. The high resolution 125 Te NMR data and the Mössbauer data for these compounds are discussed. The use of tellurium-proton couplings in high resolution 125 Te NMR spectra in assigning the resonances in mixed dialkyl ditellurides is also ...