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Determination of internuclear distances in uniformly labeled molecules by rotational-resonance solid-state NMR.

Determination of internuclear distances in uniformly labeled molecules by rotational-resonance solid-state NMR.
Determination of internuclear distances in uniformly labeled molecules by rotational-resonance solid-state NMR.
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 (13)C-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 (13)C-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.
0002-7863
2718-2722
Williamson, Philip T.F.
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a
Verhoeven, Aswin
3d5f50df-bbb5-4007-8c28-200d39f69f08
Ernst, Matthias
813ede38-ceb7-431a-b55c-da0c7fc7be5c
Meier, Beat H.
f0c14a56-63f1-4e30-9af7-6d51064ed1df
Williamson, Philip T.F.
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a
Verhoeven, Aswin
3d5f50df-bbb5-4007-8c28-200d39f69f08
Ernst, Matthias
813ede38-ceb7-431a-b55c-da0c7fc7be5c
Meier, Beat H.
f0c14a56-63f1-4e30-9af7-6d51064ed1df

Williamson, Philip T.F., Verhoeven, Aswin, Ernst, Matthias and Meier, Beat 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).

Record type: Article

Abstract

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 (13)C-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 (13)C-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.

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Published date: 2003
Organisations: Biological Sciences

Identifiers

Local EPrints ID: 45396
URI: http://eprints.soton.ac.uk/id/eprint/45396
ISSN: 0002-7863
PURE UUID: f0de60d2-9406-49d6-850a-fedab753d577
ORCID for Philip T.F. Williamson: ORCID iD orcid.org/0000-0002-0231-8640

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Date deposited: 27 Mar 2007
Last modified: 16 Mar 2024 03:53

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Contributors

Author: Aswin Verhoeven
Author: Matthias Ernst
Author: Beat H. Meier

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