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Estimation of carbon-carbon bond lengths and medium-range internuclear distances by solid-state nuclear magnetic resonance

Estimation of carbon-carbon bond lengths and medium-range internuclear distances by solid-state nuclear magnetic resonance
Estimation of carbon-carbon bond lengths and medium-range internuclear distances by solid-state nuclear magnetic resonance
We describe magic-angle-spinning NMR methods for the accurate determination of internuclear dipole-dipole couplings between homonuclear spins-1/2 in the solid state. The new sequences use symmetry principles to treat the effect of magic-angle sample-rotation and resonant radio frequency fields. The pulse-sequence symmetries generate selection rules which reduce the interference of undesirable interactions and improve the robustness of the pulse sequences with respect to chemical shift anisotropies. We show that the pulse sequences may be used to estimate distances between 13C spins in organic solids, including bond lengths in systems with large chemical shift anisotropies, such as conjugated systems. For bond-length measurements, the precision of the method is ±2 pm with a systematic overestimate of the internuclear distance by 3 ± 1 pm. The method is expected to be a useful tool for investigating structural changes in macromolecules.
angle-spinning nmr, rotating solids, rotary resonance, pulse sequences, dipolar interactions, phase transients, pair systems, l-alanine, masnmr, homonuclear
0002-7863
10628-10638
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Edén, Mattias
b51e4e79-5ef3-4d12-abcf-d08a290c1c8c
Johannessen, Ole G.
799ccc8c-a2e7-4305-a03a-2dc9f42564ef
Luthman, Henrik
662dcf74-bbdd-49d2-bac2-b84304eea393
Verdegem, Peter J.E.
72ab5611-e197-4750-9cbd-a7cdee83d67e
Lugtenburg, Johan
b920f5ab-0138-479f-88b1-f4bca6b32dad
Sebald, Angelika
0431b9a7-27aa-4a01-a1cb-7e80bd13184c
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Edén, Mattias
b51e4e79-5ef3-4d12-abcf-d08a290c1c8c
Johannessen, Ole G.
799ccc8c-a2e7-4305-a03a-2dc9f42564ef
Luthman, Henrik
662dcf74-bbdd-49d2-bac2-b84304eea393
Verdegem, Peter J.E.
72ab5611-e197-4750-9cbd-a7cdee83d67e
Lugtenburg, Johan
b920f5ab-0138-479f-88b1-f4bca6b32dad
Sebald, Angelika
0431b9a7-27aa-4a01-a1cb-7e80bd13184c
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3

Carravetta, Marina, Edén, Mattias, Johannessen, Ole G., Luthman, Henrik, Verdegem, Peter J.E., Lugtenburg, Johan, Sebald, Angelika and Levitt, Malcolm H. (2001) Estimation of carbon-carbon bond lengths and medium-range internuclear distances by solid-state nuclear magnetic resonance. Journal of the American Chemical Society, 123 (43), 10628-10638. (doi:10.1021/ja016027f).

Record type: Article

Abstract

We describe magic-angle-spinning NMR methods for the accurate determination of internuclear dipole-dipole couplings between homonuclear spins-1/2 in the solid state. The new sequences use symmetry principles to treat the effect of magic-angle sample-rotation and resonant radio frequency fields. The pulse-sequence symmetries generate selection rules which reduce the interference of undesirable interactions and improve the robustness of the pulse sequences with respect to chemical shift anisotropies. We show that the pulse sequences may be used to estimate distances between 13C spins in organic solids, including bond lengths in systems with large chemical shift anisotropies, such as conjugated systems. For bond-length measurements, the precision of the method is ±2 pm with a systematic overestimate of the internuclear distance by 3 ± 1 pm. The method is expected to be a useful tool for investigating structural changes in macromolecules.

Full text not available from this repository.

More information

Published date: 2001
Keywords: angle-spinning nmr, rotating solids, rotary resonance, pulse sequences, dipolar interactions, phase transients, pair systems, l-alanine, masnmr, homonuclear
Organisations: Chemistry

Identifiers

Local EPrints ID: 19442
URI: http://eprints.soton.ac.uk/id/eprint/19442
ISSN: 0002-7863
PURE UUID: a67cf8c2-7b36-437e-9b8f-f03f2517f6e5
ORCID for Marina Carravetta: ORCID iD orcid.org/0000-0002-6296-2104
ORCID for Malcolm H. Levitt: ORCID iD orcid.org/0000-0001-9878-1180

Catalogue record

Date deposited: 15 Feb 2006
Last modified: 29 Oct 2019 01:56

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