The CLIP/CLAP-HSQC: Pure absorptive spectra for the measurement of one-bond couplings

被引:176
作者
Enthart, Andreas [1 ]
Freudenberger, J. Christoph [1 ,2 ]
Furrer, Julien [1 ,3 ]
Kessler, Horst [1 ]
Luy, Burkhard [1 ]
机构
[1] Tech Univ Munich, Dept Chem, Munich Ctr Integrated Prot Sci, D-85747 Garching, Germany
[2] Currenta GmbH & Co, OHG, SER ANT, D-51368 Leverkusen, Germany
[3] Univ Neuchatel, Inst Chim, CH-2009 Neuchatel, Switzerland
关键词
RDCs; partial alignment; HSQC; pure absorption; IPAP;
D O I
10.1016/j.jmr.2008.03.009
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Heteronuclear residual dipolar one-bond couplings of organic molecules at natural abundance are most easily measured using t(2) coupled HSQC spectra. However, inevitably mismatched transfer delays result in phase distortions due to residual dispersive antiphase coherences in such experiments. In this article, slightly modified t2 coupled HSQC experiments with clean inphase (CLIP) multiplets are introduced which also reduce the intensities of undesired long-range cross peaks. With the corresponding antiphase (CLAP) experiment, situations where alpha and beta components overlap can be resolved for all multiplicities in an IPAP manner. A comparison of the experiments using hard pulses and shaped broadband excitation and inversion pulses on the heteronucleus is given and potential spectral artefacts are discussed in detail. (c) 2008 Elsevier Inc. All rights reserved.
引用
收藏
页码:314 / 322
页数:9
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