Measurement of Internuclear Distances by Switched Angle Spinning Nmr

TitleMeasurement of Internuclear Distances by Switched Angle Spinning Nmr
Publication TypeJournal Article
Year of Publication1994
AuthorsKolbert A.C, Grandinetti P.J, Baldwin M., Prusiner S.B, Pines A
JournalJournal of Physical Chemistry
Volume98
Issue33
Pagination7936-7938
Date PublishedAug 18
ISBN Number0022-3654
Accession NumberWOS:A1994PC61900003
Keywordsprotein
Abstract

Dipolar switched angle spinning, an NMR technique due to Terao et al. [Terao, T.; Miura H.; Saika, A, J. Chem. Phys. 1986, 85, 3816], has been used to measure C-13-C-13 distances in the solid state. The experiment involves rotation of the sample at two different angles during different periods of a two-dimensional experiment. An evolution period with off-magic-angle spinning and chemical shift refocusing, followed by detection of the signal under magic angle spinning, yields scaled Pake patterns in omega(1), correlated with their isotropic shifts in omega(2) allowing the high-resolution measurement of dipolar couplings. We demonstrate this experiment on samples of doubly C-13 labeled zinc acetate and a 14 amino acid peptide, in which we show that under optimal conditions distances of up to 5 Angstrom may be measured.

URL<Go to ISI>://WOS:A1994PC61900003
DOI10.1021/J100084a003
Short TitleMeasurement of Internuclear Distances by Switched Angle Spinning Nmr
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