Determination of internuclear distances in uniformly labeled molecules by rotational-resonance solid-state NMR
Williamson, P.T.F., Verhoeven, A., Ernst, M. and Meier, B.H. (2003) Determination of internuclear distances in uniformly labeled molecules by rotational-resonance solid-state NMR. Journal of the American Chemical Society, 125, (9), 2718-2722. (doi:10.1021/ja028210u).
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Rotational-resonance magic-angle spinning NMR experiments are frequently used to measure dipolar couplings and to determine internuclear distances. So far most measurements were performed on samples containing isolated spin pairs. Thus, extensive structure elucidation, for example in biomolecules, requires the preparation of a whole set of doubly labeled samples. Here, we describe the analysis of the rotational-resonance polarization-exchange curves obtained from a single, uniformly labeled sample. It is shown experimentally that, at a magnetic field of 14.09 T, the rotational-resonance conditions in uniformly 13C-labeled threonine are sufficiently narrow to permit the measurement of five distances between the four carbon spins with an accuracy of better than 10%. The polarization-exchange curves are analyzed using a modified two-spin model consisting of the two active spins. The modified model includes an additional offset in the final polarization, which comes from the coupling to the additional, passive, spins. The validity of this approach is experimentally verified for uniformly 13C-labeled threonine. The broader applicability of such a model is demonstrated by numerical simulations which quantify the errors as a function of the most relevant parameters in the spin system.
|Digital Object Identifier (DOI):||doi:10.1021/ja028210u|
|Subjects:||Q Science > Q Science (General)
R Medicine > R Medicine (General)
|Divisions :||University Structure - Pre August 2011 > School of Biological Sciences
|Accepted Date and Publication Date:||
|Date Deposited:||07 Aug 2008|
|Last Modified:||31 Mar 2016 12:36|
|RDF:||RDF+N-Triples, RDF+N3, RDF+XML, Browse.|
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