Accurate determination of one-bond heteronuclear coupling constants with "pure shift" broadband proton-decoupled CLIP/CLAP-HSQC experiments

István Timári, Lukas Kaltschnee, Andreas Kolmer, Ralph W. Adams, Mathias Nilsson, Christina M. Thiele, Gareth A. Morris, K. Kövér

Research output: Contribution to journalArticle

45 Citations (Scopus)

Abstract

We report broadband proton-decoupled CLIP/CLAP-HSQC experiments for the accurate determination of one-bond heteronuclear couplings and, by extension, for the reliable measurement of small residual dipolar coupling constants. The combination of an isotope-selective BIRD(d) filter module with a non-selective 1H inversion pulse is employed to refocus proton-proton coupling evolution prior to the acquisition of brief chunks of free induction decay that are subsequently assembled to reconstruct the fully-decoupled signal evolution. As a result, the cross-peaks obtained are split only by the heteronuclear one-bond coupling along the F2 dimension, allowing coupling constants to be extracted by measuring simple frequency differences between singlet maxima. The proton decoupling scheme presented has also been utilized in standard HSQC experiments, resulting in a fully-decoupled pure shift correlation map with significantly improved resolution.

Original languageEnglish
Pages (from-to)130-138
Number of pages9
JournalJournal of Magnetic Resonance
Volume239
DOIs
Publication statusPublished - Feb 2014

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Protons
broadband
protons
shift
Experiments
Isotopes
decoupling
acquisition
induction
isotopes
modules
inversions
filters
decay
pulses

Keywords

  • Broadband proton decoupling
  • F-coupled HSQC
  • IPAP
  • Pure absorption
  • RDC

ASJC Scopus subject areas

  • Nuclear and High Energy Physics
  • Biochemistry
  • Biophysics
  • Condensed Matter Physics

Cite this

Accurate determination of one-bond heteronuclear coupling constants with "pure shift" broadband proton-decoupled CLIP/CLAP-HSQC experiments. / Timári, István; Kaltschnee, Lukas; Kolmer, Andreas; Adams, Ralph W.; Nilsson, Mathias; Thiele, Christina M.; Morris, Gareth A.; Kövér, K.

In: Journal of Magnetic Resonance, Vol. 239, 02.2014, p. 130-138.

Research output: Contribution to journalArticle

Timári, István ; Kaltschnee, Lukas ; Kolmer, Andreas ; Adams, Ralph W. ; Nilsson, Mathias ; Thiele, Christina M. ; Morris, Gareth A. ; Kövér, K. / Accurate determination of one-bond heteronuclear coupling constants with "pure shift" broadband proton-decoupled CLIP/CLAP-HSQC experiments. In: Journal of Magnetic Resonance. 2014 ; Vol. 239. pp. 130-138.
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