Jb. Lambert et al., DYNAMICS OF 5-MEMBERED RINGS IN THE SOLID-STATE BY NMR-SPECTROSCOPY, Journal of the American Chemical Society, 116(14), 1994, pp. 6167-6174
The carbon-13 NMR spectra have been investigated in the solid state fo
r a number of fundamental five-membered rings and some analogous six-m
embered rings. Several of these rings freeze into a plastic phase, who
se NMR spectrum retains the symmetry of the liquid-phase spectrum. At
the plastic-to-nonplastic transition, these spectra can undergo decoal
escence to spectra characteristic of the symmetry and structure within
the solid. Motion within the solid also broadens peaks when the motio
nal frequency is comparable to the spin-lock precessional frequency. I
n the nonplastic phase, cyclopentanol exists in at least two sites, an
d possibly more, which probably result from hydrogen-bonded aggregatio
n. Cyclohexanol may exist in two such sites. Cyclopentanone exists in
two equally populated sites. 1-Methylcyclopentanol and trans-1,2-cyclo
hexanediol exist either in two equally populated sites or as a single,
unsymmetrical form. Cyclohexanone, trans-1,2-cyclohexanediol, and tet
rahydrothiophene 1-oxide appear to exist in single forms. Sulfolane ex
ists in two, unequally populated sites.