Precise Measurement of Long-Range Heteronuclear Coupling Constants by a Novel Broadband Proton-Proton-Decoupled CPMG-HSQMBC Method

被引：15

作者：

Timari, Istvan ^{[1
]}

Illyes, Tuende Z. ^{[2
]}

Adams, Ralph W. ^{[3
]}

Nilsson, Mathias ^{[3
]}

Szilagyi, Laszlo ^{[2
]}

Morris, Gareth A. ^{[3
]}

Koever, Katalin E. ^{[1
]}

机构：

[1] Univ Debrecen, Dept Inorgan & Analyt Chem, H-4032 Debrecen, Hungary

[2] Univ Debrecen, Dept Organ Chem, H-4032 Debrecen, Hungary

[3] Univ Manchester, Sch Chem, Manchester M13 9PL, Lancs, England

来源：

CHEMISTRY-A EUROPEAN JOURNAL | 2015年 / 21卷 / 08期

基金：

英国工程与自然科学研究理事会;

关键词：

HSQMBC; heteronuclear coupling constants; NMR spectroscopy; proton-proton decoupling; structure elucidation; BOND CORRELATION SPECTROSCOPY; CORRELATION NMR-SPECTROSCOPY; HSQC-TOCSY EXPERIMENTS; PURE SHIFT H-1-NMR; ACCURATE MEASUREMENT; NATURAL-ABUNDANCE; HOMONUCLEAR; RESOLUTION; SPECTRA; SENSITIVITY;

D O I：

10.1002/chem.201405535

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

A broadband proton-proton-decoupled CPMG-HSQMBC method for the precise and direct measurement of long-range heteronuclear coupling constants is presented. The Zangger-Sterk-based homodecoupling scheme reported herein efficiently removes unwanted proton-proton splittings from the heteronuclear multiplets, so that the desired heteronuclear couplings can be determined simply by measuring frequency differences between singlet maxima in the resulting spectra. The proposed pseudo-1D/2D pulse sequences were tested on nucleotides, a metal complex incorporating P heterocycles, and diglycosyl (di)selenides, as well as on other carbohydrate derivatives, for the extraction of (n)J(H-1, P-31), (n)J(H-1, Se-77), and (n)J(H-1, C-13) values, respectively.

引用

页码：3472 / 3479

页数：8

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