LR-HSQMBC versus LR-selHSQMBC: Enhancing the Observation of Tiny Long-Range Heteronuclear NMR Correlations

J Nat Prod. 2020 Apr 24;83(4):1275-1282. doi: 10.1021/acs.jnatprod.0c00058. Epub 2020 Mar 10.

Abstract

The detection of ultra-long-range (4JCH and higher) heteronuclear connectivities can complement the conventional use of HMBC/HSQMBC data in structure elucidation NMR studies of proton-deficient natural products, where two-bond and three-bond correlations are usually observed. The performance of the selHSQMBC experiment with respect to its broadband HSQMBC counterpart is evaluated. Despite its frequency-selectivity nature, selHSQMBC efficiently prevents any unwanted signal phase and intensity modulations due to passive proton-proton coupling constants typically involved in HSQMBC. As a result, selHSQMBC offers a significant sensitivity enhancement and provides pure in-phase multiplets, improving the detection levels for short- and long-range cross-peaks corresponding to small heteronuclear coupling values. This is particularly relevant for experiments optimized to small nJCH values (2-3 Hz), referred to as LR-selHSQMBC, where key cross-peaks that are not visible in the equivalent broadband LR-HSQMBC spectrum can become observable in optimum conditions.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Biological Products / chemistry*
  • Magnetic Resonance Spectroscopy / methods
  • Molecular Structure
  • Nuclear Magnetic Resonance, Biomolecular / methods*
  • Protons

Substances

  • Biological Products
  • Protons