Invited Speaker 23rd International Society of Magnetic Resonance Conference 2023

Resolution and selectivity: new methods in small molecule NMR (#168)

Gareth Morris 1
  1. University of Manchester, Manchester, GREATER MANCHESTER, United Kingdom

No matter how expensive the spectrometer, we seem never to have enough resolution. Even ‘small’ molecules can pose problems, especially in mixtures. Multiplet structure is a mixed blessing: it gives us valuable structural information, but all too often it leads to a thicket of overlapping signals. Pure shift NMR, in which we temporarily sacrifice set aside the information contained in spin-spin couplings, suppresses the effects of homonuclear couplings to leave just one peak per chemical shift – hence the name. For proton NMR this can improve resolution by up to an order of magnitude, and a wide range of pure shift methods are already in use. Some recent developments, published1-3 and unpublished, will be presented, including pure shift methods involving nuclei other than 1H.

Selective excitation methods offer another route to improve resolution, but once again multiplet structure poses problems: ideally we would like to excite a single chemical shift, not a single frequency. The GEMSTONE variation on chemical shift selective filtration (CSSF)4 allows us to do this particularly efficiently, opening up a range of ultraselective 1D analogues of 2D experiments.5-7 Finally, data processing methods can both optimise the precision of measurements and take us beyond normal instrumental limits on resolution.

  1. Mycroft et al., ChemPhysChem 23, e202200495 (2022).
  2. Smith et al., Anal. Chem. 94, 12757 (2022).
  3. Smith et al., Org. Biomol. Chem. 21, 2984-3990 (2023).
  4. Robinson et al., J. Magn. Reson. 170, 97 (2004).
  5. Kiraly et al., Angew. Chem. Int. Ed. 60, 666 (2021); Chem. Commun. 57, 2368 (2021).
  6. Gates et al., Chem. Commun. 59, 5854 (2023).
  7. Taylor et al., Chem. Commun. 59, 6734-6737 (2023).