1,2-Dichlorotetrafluorocyclobutene (A) and 1,2-dichlorohexafluorocylopentene-1 (B) were reacted with triazamacrocyclic amines (1,4,8-triazacycloundecane (1) and 1,5,9-triazacyclo-dodecane (2)) at 80 degrees C in the presence of stoichiometric amounts of triethylamine in benzene. Cycloalkene A formed a 2 : 1 product 3 with 1 and a 3:1 product 4 with 2. Cycloalkene B formed only 2:1 products 5 and 6 with 1 and 2, respectively. The crystal structures of 3 and 4 were determined by single-crystal X-ray diffraction.