Unambiguous assignment of the resonances of different diastereomers in a nonracemic mixture is possible with (1)H-decoupled (2)H NMR spectroscopy in a chiral liquid crystalline solvent. This is demonstrated with, for example, the alpha,alpha'-dideuterated diol shown in the picture. Even diastereomers with centers of chirality up to nine bonds apart can be discriminated.
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