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Carbon-13 Heteronuclear Longitudinal Spin Relaxation for Geometrical (and Stereochemical) Determinations in Small or Medium Size Molecules

Abstract : Owing to an extremely abundant literature making use of spin relaxation for structural studies, this review is limited to carbon-13 spectroscopy, to small or medium size molecules, to stereochemical and preferably geometrical determinations. The parameter of choice is evidently the Nuclear Overhauser effect (NOE) because it depends exclusively on the dipolar interaction mechanism, thus on 1/r6, where r is the distance between the two interacting spins. However, it depends also on the dynamical features of the system under investigation which must be characterized prior to any attempt for obtaining geometrical or stereochemical information. Therefore, this review is devoted not only to 1H–13C NOE but, more generally, to 13C longitudinal relaxation. After comprehensive theoretical developments, experimental methods presently available will be presented. The latter include the usual gated decoupling experiment and pulse experiments of the HOESY (Heteronuclear Overhauser Effect SpectroscopY) family. These pulse experiments, which imply carbon-13 observation, can be one-dimensional, selective one-dimensional or two-dimensional. The emphasis will be put on the interpretation which is different according to the occurrence or not of extreme narrowing conditions. Along with a literature survey, some selected examples will be presented in detail in order to illustrate the potentiality of the method.
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Daniel Canet, Sabine Bouguet-Bonnet, Sébastien Leclerc, Mehdi Yemloul. Carbon-13 Heteronuclear Longitudinal Spin Relaxation for Geometrical (and Stereochemical) Determinations in Small or Medium Size Molecules. Annual Reports on NMR Spectroscopy, Elsevier, 2011, 74, pp.89-123. ⟨10.1016/B978-0-08-097072-1.00002-9⟩. ⟨hal-01482005⟩

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