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Structural analysis of uniformly (13)C-labelled solids from selective angle measurements at rotational resonance

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Structural analysis of uniformly (13)C-labelled solids from selective angle measurements at rotational resonance. / Patching, Simon G; Edwards, Rachel; Middleton, David A.
In: June 2002. ISSN 1460-4582, Vol. 199, No. 2, 08.2009, p. 242-6.

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Patching SG, Edwards R, Middleton DA. Structural analysis of uniformly (13)C-labelled solids from selective angle measurements at rotational resonance. June 2002. ISSN 1460-4582. 2009 Aug;199(2):242-6. doi: 10.1016/j.jmr.2009.05.002

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Patching, Simon G ; Edwards, Rachel ; Middleton, David A. / Structural analysis of uniformly (13)C-labelled solids from selective angle measurements at rotational resonance. In: June 2002. ISSN 1460-4582. 2009 ; Vol. 199, No. 2. pp. 242-6.

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@article{9b45dffe89734cce92ed606946ff768a,
title = "Structural analysis of uniformly (13)C-labelled solids from selective angle measurements at rotational resonance",
abstract = "We demonstrate that individual H-C-C-H torsional angles in uniformly labelled organic solids can be estimated by selective excitation of (13)C double-quantum coherences under magic-angle spinning at rotational resonance. By adapting a straightforward one-dimensional experiment described earlier [T. Karlsson, M. Eden, H. Luhman, M.H. Levitt, J. Magn. Reson. 145 (2000) 95-107], a double-quantum filtered spectrum selective for Calpha and Cbeta of uniformly labelled L-[(13)C,(15)N]valine is obtained with 25% efficiency. The evolution of Calpha-Cbeta double-quantum coherence under the influence of the dipolar fields of bonded protons is monitored to provide a value of the Halpha-Calpha-Cbeta-Hbeta torsional angle that is consistent with the crystal structure. In addition, double-quantum filtration selective for C6 and C1' of uniformly labelled [(13)C,(15)N]uridine is achieved with 12% efficiency for a (13)C-(13)C distance of 2.5A, yielding a reliable estimate of the C6-H and C1'-H projection angle defining the relative orientations of the nucleoside pyrimidine and ribose rings. This procedure will be useful, in favourable cases, for structural analysis of fully labelled small molecules such as receptor ligands that are not readily synthesised with labels placed selectively at structurally diagnostic sites.",
keywords = "Algorithms, Carbon Isotopes, Computer Simulation, Magnetic Resonance Spectroscopy, Models, Chemical, Rotation, Staining and Labeling",
author = "Patching, {Simon G} and Rachel Edwards and Middleton, {David A}",
year = "2009",
month = aug,
doi = "10.1016/j.jmr.2009.05.002",
language = "English",
volume = "199",
pages = "242--6",
journal = "June 2002. ISSN 1460-4582",
issn = "0893-3200",
publisher = "American Psychological Association Inc.",
number = "2",

}

RIS

TY - JOUR

T1 - Structural analysis of uniformly (13)C-labelled solids from selective angle measurements at rotational resonance

AU - Patching, Simon G

AU - Edwards, Rachel

AU - Middleton, David A

PY - 2009/8

Y1 - 2009/8

N2 - We demonstrate that individual H-C-C-H torsional angles in uniformly labelled organic solids can be estimated by selective excitation of (13)C double-quantum coherences under magic-angle spinning at rotational resonance. By adapting a straightforward one-dimensional experiment described earlier [T. Karlsson, M. Eden, H. Luhman, M.H. Levitt, J. Magn. Reson. 145 (2000) 95-107], a double-quantum filtered spectrum selective for Calpha and Cbeta of uniformly labelled L-[(13)C,(15)N]valine is obtained with 25% efficiency. The evolution of Calpha-Cbeta double-quantum coherence under the influence of the dipolar fields of bonded protons is monitored to provide a value of the Halpha-Calpha-Cbeta-Hbeta torsional angle that is consistent with the crystal structure. In addition, double-quantum filtration selective for C6 and C1' of uniformly labelled [(13)C,(15)N]uridine is achieved with 12% efficiency for a (13)C-(13)C distance of 2.5A, yielding a reliable estimate of the C6-H and C1'-H projection angle defining the relative orientations of the nucleoside pyrimidine and ribose rings. This procedure will be useful, in favourable cases, for structural analysis of fully labelled small molecules such as receptor ligands that are not readily synthesised with labels placed selectively at structurally diagnostic sites.

AB - We demonstrate that individual H-C-C-H torsional angles in uniformly labelled organic solids can be estimated by selective excitation of (13)C double-quantum coherences under magic-angle spinning at rotational resonance. By adapting a straightforward one-dimensional experiment described earlier [T. Karlsson, M. Eden, H. Luhman, M.H. Levitt, J. Magn. Reson. 145 (2000) 95-107], a double-quantum filtered spectrum selective for Calpha and Cbeta of uniformly labelled L-[(13)C,(15)N]valine is obtained with 25% efficiency. The evolution of Calpha-Cbeta double-quantum coherence under the influence of the dipolar fields of bonded protons is monitored to provide a value of the Halpha-Calpha-Cbeta-Hbeta torsional angle that is consistent with the crystal structure. In addition, double-quantum filtration selective for C6 and C1' of uniformly labelled [(13)C,(15)N]uridine is achieved with 12% efficiency for a (13)C-(13)C distance of 2.5A, yielding a reliable estimate of the C6-H and C1'-H projection angle defining the relative orientations of the nucleoside pyrimidine and ribose rings. This procedure will be useful, in favourable cases, for structural analysis of fully labelled small molecules such as receptor ligands that are not readily synthesised with labels placed selectively at structurally diagnostic sites.

KW - Algorithms

KW - Carbon Isotopes

KW - Computer Simulation

KW - Magnetic Resonance Spectroscopy

KW - Models, Chemical

KW - Rotation

KW - Staining and Labeling

U2 - 10.1016/j.jmr.2009.05.002

DO - 10.1016/j.jmr.2009.05.002

M3 - Journal article

C2 - 19487142

VL - 199

SP - 242

EP - 246

JO - June 2002. ISSN 1460-4582

JF - June 2002. ISSN 1460-4582

SN - 0893-3200

IS - 2

ER -