The first trlchothecene, tnchothecln was isolated in 1948 by Freeman and Morrison' At that time, the sophisticated spectroscoprc techniques used today for the characterization of compounds were not available This IS especially true of nuclear magnetic resonance spectroscopy (NMR), which only became a commercial reality in the late 1950s The data produced at 60 and later 100 MHz for proton ('H) resonance were limited, comprising mainly of chemical shifts and some coupling constants With the advent in the 1970s of Fourier Transform NMR and superconducting magnets, which enable fields of up to 600 MHz to be achieved, NMR is now the principal technique employed forthedeterminatlon of the structureoftnchothecenes, including their stereochemistry and conformation During the past two decades, the tnchothecenes have emerged as importantmycotoxins due to their toxic effects on animals and humans Further interest was stimulated in part, by the heavy contamination of cereal crops In North America with 4-deoxynlvalenol in the 1980s and the resulting health hazard' The trlchothecenes are mevalonate-derived sesquiterpenes, which have in common atncyclic nng system. They differ in the degree of oxidation at the ring carbon atoms, C-3, C-4, C-7, C-8 and C-15 and the extent and type of esterlflcation of the hydroxyl moletles. Including the acylated derrvatlves, there are over 90 compounds in this class In additlon,there are a growing number of trichothecene-related compounds which are derived from the common intermediate trlchodlene, e g. sambuclnol, sambucoln and several apotnchothecene denvatlves The structures of these compounds are shown in Figure 1 NMR spectral assignments of proton chemical shifts and coupling constants in the older literature were based on single frequency off-resonance proton decoupling. This technique together with spin-lattice relaxatlontimemeasurements and biosynthetic enrichment studies were used to assign the spectra of trichodermin', trichodermol', and trichothecin' The newer techniques for establishing carbon resonance assignments include Distortionless Enhanced Polanzation Transfer (DEPT) and 'H/13C heteronuclear correlation spectra (HETCOR) Similarly, for proton assignments, 2D or 'H/'H homonuclear correlated spectra (COSY) are now used as well as nuclear Overhauser effect (NOE) difference spectra Although the 'H and 13C resonances for