PSYCHE CPMG-HSQMBC: An NMR Spectroscopic Method for Precise and Simple Measurement of Long-Range Heteronuclear Coupling Constants

Among the NMR spectroscopic parameters, long‐range heteronuclear coupling constants convey invaluable information on torsion angles relevant to glycosidic linkages of carbohydrates. A broadband homonuclear decoupled PSYCHE CPMG–HSQMBC method for the precise and direct measurement of multiple‐bond he...

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Bibliographic Details
Published in:Chemistry : a European journal 2015-09, Vol.21 (40), p.13939-13942
Main Authors: Timari, István, Szilagyi, László, Kover, Katalin E
Format: Article
Language:English
Subjects:
Broadband
broadband homonuclear decoupling
Carbohydrates
Chemistry
Constants
Couplings
HSQMBC
Joining
long-range heteronuclear coupling
Maxima
NMR
NMR spectroscopy
Nuclear magnetic resonance
Rangefinding
Spectroscopy
Splitting
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Summary:Among the NMR spectroscopic parameters, long‐range heteronuclear coupling constants convey invaluable information on torsion angles relevant to glycosidic linkages of carbohydrates. A broadband homonuclear decoupled PSYCHE CPMG–HSQMBC method for the precise and direct measurement of multiple‐bond heteronuclear couplings is presented. The PSYCHE scheme built into the pulse sequence efficiently eliminates unwanted proton–proton splittings from the heteronuclear multiplets so that the desired heteronuclear couplings can be determined simply by measuring frequency differences between peak maxima of pure antiphase doublets. Moreover, PSYCHE CPMG–HSQMBC can provide significant improvement in sensitivity as compared to an earlier Zangger–Sterk‐based method. Applications of the proposed pulse sequence are demonstrated for the extraction of nJ(1H,77Se) and nJ(1H,13C) values, respectively, in carbohydrates; further extensions can be envisioned in any J‐based structural and conformational studies. A PSYCHE sequence incorporated in the CPMG–HSQMBC NMR experiment for broadband homonuclear decoupling efficiently removes undesired proton–proton splittings from heteronuclear multiplets. This method allows long‐range heteronuclear couplings of interest to be determined simply by measuring frequency differences between maxima of pure antiphase doublets.
ISSN:0947-6539
1521-3765
DOI:10.1002/chem.201502641