Polyphenylacetylenes were prepared using ferric acetylacetonate and (i‐Bu)2AlH, RhCl[(C6H5)3P]3 and thermal initiation. Color, infrared spectra, softening temperatures, ultraviolet fluorescence, solubility, and crystallinity are described. A method is presented for assigning to these three macromolecular species predominantly cis, trans, and cis–trans copolymer structures, respectively. The dominantly cis polymer is believed to form in a transoid conformation which can easily be transformed to a more helical arrangement which exhibits a degree of crystallinity. Pyridine promotes the isomerization of cis to trans structure. The rhodium phosphine is thought to effect chain growth by repeated additions of the acetylenic CH of monomer across a terminal triple bond. Phenylacetylene thus behaves as a bifunctional molecule in this system. Color, polymer conformation, and crystallinity appear to be strongly interrelated.
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