Group 12 mercury(ii) polyyne polymers containing derivatized benzene spacers were prepared in good yields using Hagihara’s dehydrohalogenation reaction of HgCl₂ with HC≡C(C₆H₂R)₂C≡CH (R = 4,5-dioctyloxy, 2,5-dihexadecyloxy) at room temperature in a basic medium. The structures of these polymers were confirmed by standard spectroscopic methods and their luminescent properties were examined. Our investigations indicate that two polymers exhibit different luminescence properties due to different position of the substituents on the benzene spacer.