The synthesis of the nickel dialkynyl complex Ni(C=C-C6H4-C=CH)(2)(PPh(3))(2) and of the corresponding polyyne polymer containing nickel in the main chain -[Ni(PPh(3))(2)-C=C-C6H4-C=C-](n) are described and discussed. A new mixed solvent system DMSO/HNEt(2) and homogeneous step-wise condensation method used for their synthesis are presented for the first time. The Ni-polyyne polymer obtained is dark yellow powder and soluble in THF or CH2Cl2. Its (M) over bar(w) is about 10(4), and the MWD is less than 2. Both the prepared complex and polymer have been characterized by IR, UV, H-1-NMR, and DTA. Preliminary results on photoluminesence of nickel polyyne polymers are present.