Accurate determination of one-bond heteronuclear coupling constants with %26quot;pure shift%26quot; broadband proton-decoupled CLIP/CLAP-HSQC experiments

作者：Timari Istvan; Kaltschnee Lukas; Kolmer Andreas; Adams Ralph W; Nilsson Mathias; Thiele Christina M; Morris Gareth A; Koever Katalin E

来源：Journal of Magnetic Resonance, 2014, 239: 130-138.

DOI：10.1016/j.jmr.2013.10.023

• Broadband proton decoupling
• F-2-coupled HSQC
• Pure absorption
• IPAP
• RDC

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 nonselective H-1 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 F-2 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.

• 出版日期2014-2