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Two new functional polyacetylenes bearing different azobenzene group, -{ HC=C[azo-N(CH3)CH2CH2OH] } n-, [poly(EHAB); azo = 4,4'-azobenzene] and - { HC=C[azo-N(CH3)CH2CH2OCOC3H7]}n-, [poly(EEAB)]} were prepared by [Rh(nbd)Cl]2-Et3N catalysts. Poly(EHAB