TY - JOUR
T1 - Accurate determination of one-bond heteronuclear coupling constants with "pure shift"' broadband proton-decoupled CLIP/CLAP-HSQC experiments
AU - Timari, Istvan
AU - Kaltschnee, Lukas
AU - Kolmer, Andreas
AU - Adams, Ralph W.
AU - Nilsson, Lars Mathias
AU - Thiele, Christina M.
AU - Morris, Gareth A.
AU - Kövér, Katalin E.
PY - 2014/2
Y1 - 2014/2
N2 - 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.
AB - 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.
U2 - 10.1016/j.jmr.2013.10.023
DO - 10.1016/j.jmr.2013.10.023
M3 - Journal article
C2 - 24368124
SN - 1090-7807
VL - 239
SP - 130
EP - 138
JO - Journal of Magnetic Resonance
JF - Journal of Magnetic Resonance
ER -