Predicting 19 F NMR Chemical Shifts: A Combined Computational and Experimental Study of a Trypanosomal Oxidoreductase-Inhibitor Complex

Angew Chem Int Ed Engl. 2020 Jul 27;59(31):12669-12673. doi: 10.1002/anie.202000539. Epub 2020 May 25.

Abstract

The absence of fluorine from most biomolecules renders it an excellent probe for NMR spectroscopy to monitor inhibitor-protein interactions. However, predicting the binding mode of a fluorinated ligand from a chemical shift (or vice versa) has been challenging due to the high electron density of the fluorine atom. Nonetheless, reliable 19 F chemical-shift predictions to deduce ligand-binding modes hold great potential for in silico drug design. Herein, we present a systematic QM/MM study to predict the 19 F NMR chemical shifts of a covalently bound fluorinated inhibitor to the essential oxidoreductase tryparedoxin (Tpx) from African trypanosomes, the causative agent of African sleeping sickness. We include many protein-inhibitor conformations as well as monomeric and dimeric inhibitor-protein complexes, thus rendering it the largest computational study on chemical shifts of 19 F nuclei in a biological context to date. Our predicted shifts agree well with those obtained experimentally and pave the way for future work in this area.

Keywords: African sleeping sickness; NMR spectroscopy; covalent inhibitors; quantum chemistry; structural biology.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Enzyme Inhibitors / chemistry*
  • Enzyme Inhibitors / metabolism
  • Fluorine / chemistry
  • Mutation
  • Nuclear Magnetic Resonance, Biomolecular / methods*
  • Protein Binding
  • Protozoan Proteins / antagonists & inhibitors
  • Protozoan Proteins / chemistry
  • Protozoan Proteins / genetics
  • Protozoan Proteins / metabolism
  • Pyrimidinones / chemistry*
  • Pyrimidinones / metabolism
  • Thiophenes / chemistry*
  • Thiophenes / metabolism
  • Thioredoxins / antagonists & inhibitors
  • Thioredoxins / chemistry*
  • Thioredoxins / genetics
  • Thioredoxins / metabolism
  • Trypanocidal Agents / chemistry*
  • Trypanocidal Agents / metabolism
  • Trypanosoma brucei brucei / enzymology

Substances

  • Enzyme Inhibitors
  • Protozoan Proteins
  • Pyrimidinones
  • Thiophenes
  • Trypanocidal Agents
  • tryparedoxin
  • Fluorine
  • Thioredoxins