pi-Conjugated poly(aryleneethynylene)s consisting of N,N'-bis(salicylidene)-1,2-phenylenediamine (salophen) units (Poly-1-Poly-3) and salophen nickel complex units (Poly-1-Ni) were prepared in high yields by the palladium-catalyzed polycondensation of H--Ar--H (Ar = fluorene or 2,5-dialkoxy-p phenylene) with dibromo compounds of salophen (Br-2-Salophen) and its nickel complex (Br-2-Salophen-Ni), respectively The Ni free polymers (Poly-1-Poly-3) showed good solubility in CHCl3 and THF, had high thermal stability, and exhibited number average molecular weights (M-n) of 9200-14000 in GPC analysis The UV-vis spectra of the polymers showed pi-pi* transition peaks at about 420 nm which was comparable to those of poly(p-phenyleneethynylene)s The UV-vis spectrum of Poly-1-Ni exhibited additional intermediate and small peaks at about 480 and 600 nm, which were assigned to a charge transfer (CT) electronic transition and a d-d transition, respectively The complexation of Poly-1 with Ni2+ proceeded clearly and quantitatively to give Poly-1-Ni, as monitored by UV-vis spectroscopy Both the NI-free and Ni containing polymers were electrochemically active and CV (cyclic volammetry) scans of the polymers showed a reduction peak of the salophene unit at approximately -2 2 V vs Ag+/Ag and an oxidation peak of the salophene unit at about 0 8 V vs Ag+/Ag