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Crystallization during polymerization of polydiphenylsilylene has been accomplished. Best results are obtained by initial thermal polymerization to the amorphous macromolecule. The macromolecules are then decomposed and repolymerized by sublimation. Macroscopic extended‐chain single crystals are produced. The polymer crystals, once molten, will not recrystallize. Their initial characterization is described using infrared, Raman, ultraviolet, and nuclear magnetic resonance spectroscopy. X‐ray and thermal analysis data are also given.
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Lee et al. (1977) studied this question.
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