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

The CLIP/CLAP-HSQC: Pure absorptive spectra for the measurement of one-bond couplings
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DOI:
10.1016/j.jmr.2008.03.009
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发表时间:
2008-06-01
影响因子:
2.2
通讯作者:
Luy, Burkhard
Luy, Burkhard
中科院分区:
化学3区
文献类型:
--
作者:
Enthart, Andreas;Freudenberger, J. Christoph;Luy, Burkhard

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在自然丰度下,有机分子的杂原子残余偶极单键耦合最容易用t(2)耦合HSQC光谱测量。然而,不可避免地失配的传输延迟导致相位失真,由于残留的色散反相相干在这样的实验中。在这篇文章中,稍微修改的t2耦合HSQC实验与清洁同相(CLIP)多重峰也减少了不需要的长程交叉峰的强度。通过相应的反相(CLAP)实验,可以以IPAP方式解决α和β分量重叠的情况。给出了使用硬脉冲和整形宽带激发和反转脉冲的实验的比较,并详细讨论了潜在的光谱伪影。(c)2008年爱思唯尔公司All rights reserved.
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.