The tripledecker complexes, bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,2,3,4-tetraalkylcyclobutadiene$)dicobalt were produced by the reaction of Jonas reagent with 2-hexyne and 3-hexyne in the maximum yield (above 50%) when they were reacted in eq-molar amounts at room temperature. A tripledecker complex, bis-${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,2,3,4-tetraethyl cyclobutadiene$)dicobalt(13) was isomerized to (${\eta}^5-cyclopentadienyl)cobaltacyclopentadiene-{\mu}-({\eta}^4-2,4-cobaltacyclopentadiene$)(${\eta}^5-cyclopentadienyl$)cobalt(15) on reacting with 3-hexyne at room temperature. Another tripledecker complex, bis-(${\eta}^5-cyclopentadienyl)-{\mu}-({\eta}^4-1,3-dimethyl-2,4-dipropyl cyclobutadiene$)dicobalt(14) was decomposed to give 1,3,5-trimethyl-2,4,6-tripropylbenzene through an intermediate complex by the reaction of 2-hexyne.