Measurement of internuclear distances by switched angle spinning NMR
- Lawrence Berkeley Lab., CA (United States) Univ. of California, Berkeley, CA (United States)
- Lawrence Berkeley Lab., CA (United States) Univ. of California, Berkeley, CA (United States) Univ. of California, San Francisco, CA (United States)
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 [sup 13]C-[sup 13]C 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][sub 1], correlated with their isotropic shifts in [omega][sub 2] allowing the high-resolution measurement of dipolar couplings. We demonstrate this experiment on samples of doubly [sup 13]C 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. 21 refs., 4 figs.
- DOE Contract Number:
- AC03-76SF00098
- OSTI ID:
- 6914819
- Journal Information:
- Journal of Physical Chemistry; (United States), Journal Name: Journal of Physical Chemistry; (United States) Vol. 98:33; ISSN JPCHAX; ISSN 0022-3654
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400102 -- Chemical & Spectral Procedures
400201* -- Chemical & Physicochemical Properties
ACETATES
CARBON 13
CARBON ISOTOPES
CARBOXYLIC ACID SALTS
DISTANCE
EVEN-ODD NUCLEI
INTERATOMIC DISTANCES
ISOTOPES
LABELLED COMPOUNDS
LIGHT NUCLEI
MAGNETIC RESONANCE
NUCLEAR MAGNETIC RESONANCE
NUCLEI
ORGANIC COMPOUNDS
PEPTIDES
POLYPEPTIDES
PROTEINS
RESONANCE
STABLE ISOTOPES
ZINC COMPOUNDS