A new rotor-synchronized carbon-13 three-dimensional magic angle spinning NMR experiment for the extraction of orientational distribution functions from partially ordered solid materials is presented. Problems with overlap of two-dimensional spinning sideband patterns inherent in earlier methods are overcome by extension to three dimensions, allowing the degree of order for each resolvable carbon site to be measured. The new technique is demonstrated on a frozen smectic liquid-crystalline side group polymer which shows an order gradient from the aligned mesogen to the disordered polymer main chain.
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Titman et al. (1993) studied this question.
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