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宽带同核去耦HSQMBC方法

Broadband homonuclear decoupled HSQMBC methods.

作者信息

Timári István, Kövér Katalin E

机构信息

Department of Inorganic and Analytical Chemistry, University of Debrecen, Egyetem tér 1, H-4032, Debrecen, Hungary.

Department of Chemistry and Biochemistry, The Ohio State University, 100 West 18th Avenue, 43210, Columbus, OH, USA.

出版信息

Magn Reson Chem. 2018 Oct;56(10):910-917. doi: 10.1002/mrc.4700. Epub 2018 Jan 9.

Abstract

Long-range heteronuclear coupling constants convey invaluable information for stereochemical and conformational analysis of molecules from synthetic and natural origin. Here, we report a real-time Zangger-Sterk CPMG-HSQMBC method for the precise and direct measurement of multiple-bond heteronuclear couplings. It is demonstrated that the real-time acquisition strategy combined with multiple slice selective excitation can provide substantial improvement in sensitivity (or reduction of experimental time) as compared to other variants of broadband homonuclear decoupled HSQMBC methods published previously. Scope and limitations of the different strategies applied for decoupling are reviewed. Moreover, practical guidelines for the choice of the most appropriate method are also presented. Applications are given on a metal complex incorporating P-heterocycles and two diglycosyl-selenides for the extraction of J( H, P) and J( H, Se), respectively.

摘要

远程异核耦合常数为来自合成和天然来源的分子的立体化学和构象分析提供了宝贵信息。在此,我们报告了一种用于精确直接测量多键异核耦合的实时臧格-斯特克CPMG-HSQMBC方法。结果表明,与先前发表的宽带同核去耦HSQMBC方法的其他变体相比,实时采集策略与多层选择性激发相结合可显著提高灵敏度(或减少实验时间)。本文综述了用于去耦的不同策略的范围和局限性。此外,还给出了选择最合适方法的实用指南。文中给出了该方法在含磷杂环的金属配合物和两种二糖基硒化物上的应用,分别用于提取J(H,P)和J(H,Se)。

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