Department of Inorganic and Analytical Chemistry, University of Debrecen, Egyetem tér 1, H-4032 Debrecen, Hungary.
Clemens-Schöpf-Institut für Organische Chemie und Biochemie, Technische Universität Darmstadt, Alarich-Weiss-Straße 4, D-64287 Darmstadt, Germany.
J Magn Reson. 2014 Feb;239:130-8. doi: 10.1016/j.jmr.2013.10.023. Epub 2013 Nov 14.
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 (1)H 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.
我们报告了宽带质子去耦 CLIP/CLAP-HSQC 实验，用于准确确定单键异核耦合，并且可以扩展用于可靠测量小的残余偶极耦合常数。采用具有非选择性（1）H 反转脉冲的同位素选择性 BIRD((d))滤波器模块，在获得随后组装以重建完全去耦信号演化的短自由感应衰减块之前，重新聚焦质子-质子耦合演化。结果，所得到的交叉峰仅沿着 F2 维度由异核单键耦合分裂，允许通过测量单峰之间的简单频率差来提取耦合常数。所提出的质子去耦方案也已用于标准 HSQC 实验，导致具有显著提高分辨率的完全去耦纯位移相关图。
