Determination of heteronuclear long-range couplings to heteronuclei in natural abundance by two- and three-dimensional NMR spectroscopy
Determination of heteronuclear long-range couplings to heteronuclei in natural abundance by two- and three-dimensional NMR spectroscopy
复制标题
通过二维和三维核磁共振波谱测定自然丰度中异核与异核的长程耦合
DOI：
--
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发表时间：
1991
影响因子：
2.7
通讯作者：
H. Kessler
中科院分区：
文献类型：
--
作者：
P. Schmieder;M. Kurz;H. Kessler
总结一种方法，以确定杂原子长程耦合碳和氮在自然丰度，并适用于两个环六肽和肽大环内酯FK 506。该方法适用于含质子的异质核。通过在二维或三维实验中引入异质半滤波器，在没有异质解耦的情况下执行时，光谱表现出E.COSY图案。用环（-Ala-Ala-Ala-Pro-Ala-Pro-）α ~（13）C-ω I半滤TOCSY谱，得到3 J（HN-Cβ）耦合常数，可用于消除3 J（HN-Hα）中夹角测定的模糊性。应用Incyclo（-d-Pro-Phe-Phe-Lys（Z）-Trp-Phe-）a15 N-ω I-半过滤TOCSY通过3 J（H → N）分别分配非对映异构体β-亚甲基质子。在FK 506中，使用没有杂原子去耦的3D-HMQC-TOCSY来获得许多与碳的杂原子耦合常数。这些值已被应用于分配的非对映异构亚甲基质子和二面角的测定在环状部分的分子。
SummaryA method to determine heteronuclear long-range couplings to carbon and nitrogen at natural abundance is presented and applied to two cyclic hexapeptides and the peptidomacrolide FK506. The method is applicable for proton-bearing heteronuclei. By introduction of heteronuclear half-filters in two- or three-dimensional experiments the spectra exhibit an E.COSY pattern when executed without heteronuclear decoupling. The extraction of the heteronuclear coupling constants is therefore independent of linewidth.Incyclo(-Ala-Ala-Ala-Pro-Ala-Pro-) a13C-ωI-half-filtered TOCSY spectrum yields the3J(HN-Cβ) coupling constant, which can be used to remove ambiguity in the ϖ angle determination from3J(HN-Hα). Incyclo(-d-Pro-Phe-Phe-Lys(Z)-Trp-Phe-) a15N-ωI-half-filtered TOCSY was applied to individually assign the diastereotopic β-methylene protons via the3J(H∇-N). In FK506 a 3D-HMQC-TOCSY without heteronuclear decoupling is used to obtain a number of heteronuclear coupling constants to carbons. These values have been applied for the assignment of diastereotopic methylene protons and determination of dihedral angles in the cyclic portion of the molecule.
影响因子：
56.9
作者：
SCHREIBER, SL
通讯作者：
SCHREIBER, SL
通过多核核磁共振测定反式 Ac-Asn-Pro-Tyr-NHMe 和反式 Ac-Tyr-Pro-Asn-NHMe 在二甲基亚砜和水中的构象特性。
DOI：
10.1111/j.1399-3011.1986.tb01052.x
发表时间：
1986
期刊：
International journal of peptide and protein research
影响因子：
--
作者：
Stimson,ER;Meinwald,YC;Montelione,GT;Scheraga,HA
通讯作者：
Scheraga,HA