Novel symmetrical 3,6-bis [(25,26,27-tripropoxy-28-(3-(4-iodophenyl)propoxy)-p-tert -butyl calix [4]arene ethynyl]-9H-fluoren-9-one with a cone conformation was synthesized by palladium-catalyzed coupling of (25,26,27-tripropoxy-28-(3-(4-iodophenyl)propoxy)-p -tert -butyl calix [4]arene and 3,6-diethynyl-9H-fluoren-9-one. Its structure was confirmed by FT-IR, 1 H-NMR, and 13 C-NMR spectroscopy, and elemental analysis and positive ion FAB mass spectrometry.