Satellite-transition MAS NMR of spin I=3/2, 5/2, 7/2, and 9/2 nuclei: sensitivity, resolution, and practical implementation

Ashbrook, S.E. and Wimperis, S. (2002) Satellite-transition MAS NMR of spin I=3/2, 5/2, 7/2, and 9/2 nuclei: sensitivity, resolution, and practical implementation. Journal of Magnetic Resonance, 156(2), pp. 269-281. (doi:10.1006/jmre.2002.2557)

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Publisher's URL: http://dx.doi.org/10.1006/jmre.2002.2557

Abstract

The satellite-transition MAS (STMAS) experiment offers an alternative approach to established methods such as dynamic angle spinning (DAS), double rotation (DOR), and multiple-quantum MAS (MQMAS) for obtaining high-resolution NMR spectra of half-integer quadrupolar nuclei. Unlike the multiple-quantum experiment, STMAS involves two-dimensional correlation of purely single-quantum coherences; satellite transitions in t1 (or F1) and the central transition in t2 (or F2). To date, STMAS has primarily been demonstrated for nuclei with spin quantum numbers I=3/2 and, to a lesser extent, I>5/2. However, many chemically relevant nuclei possess I>3/2, such as 17O and 27Al (both I=5/2), 59Co (I=7/2), and 93Nb (I=9/2). Here, we discuss the application of STMAS to nuclei with spin quantum numbers from I=3/2 to 9/2. First, we consider the practical implementation of the STMAS experiment using 87Rb (I=3/2) NMR as an example. We then extend the discussion to include nuclei with higher spin quantum numbers, demonstrating 27Al, 45Sc (I=7/2), 59Co, and 93Nb STMAS experiments on both crystalline and amorphous samples. We also consider the possibility of experiments involving satellite transitions other than mI=±1/2↔±3/2 and, using 93Nb NMR, demonstrate the correlation of all single-quantum satellite transitions up to and including mI=±7/2↔±9/2. The absolute chemical shift scaling factors in these experiments are discussed, as are the implications for isotropic resolution.

Item Type:Articles
Status:Published
Refereed:Yes
Glasgow Author(s) Enlighten ID:Wimperis, Professor Stephen
Authors: Ashbrook, S.E., and Wimperis, S.
College/School:College of Science and Engineering > School of Chemistry
Journal Name:Journal of Magnetic Resonance
Publisher:Academic Press
ISSN:1090-7807
ISSN (Online):1096-0856
Published Online:06 August 2002

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