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1.Introduction We have demonstrated that the rhodium norbornadiene:[Rh(nbd)C1]2 (nbd=norbomadien) can be used as the most useful catalyst for the highly stereoregular polymerization of mono-substituted acetylenes.The resulting polymer has helical cis-tansoid form able to construct a pseudohexagonal structure (columnar) as a self-assemble in the solid phase.In this report,poly(alkyl propiolate)s:PAP having a normal (PnAP;1,3) and a branched alkyl chain (P2AP;2,4) were synthesized and their structures in solution was also studied in detail by conventional analytical methods.