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J Biomol NMR. 1993 Jul;3(4):487-93.

A simple and sensitive experiment for measurement of JCC couplings between backbone carbonyl and methyl carbons in isotopically enriched proteins.

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Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, MD 20892.


A simple 2D difference experiment is described that allows quantitative measurement of 13C-13C J couplings between backbone carbonyl and side-chain carbons. Precise 3JCC values were measured from data recorded in just 2 h for a 1-mM solution of the 20-kD complex between the protein calmodulin and a 26-residue synthetic peptide. The J couplings aid in determining the chi 1 angles of valine, isoleucine and threonine residues, and in making stereospecific assignments of the Val C gamma methyl groups. Error analysis indicates that the uncertainty in the derived J couplings is generally less than ca. 0.3 Hz.

[Indexed for MEDLINE]

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