The macrotricycles 15,16-diphenyl-1,5,8,12-tetraazatricyclo[10,2,1,1 5,8 ]hexadecane 2′ and 15,16-dipyridin-2-yl-1,4,8,11-tetraazatricyclo[9,3,1,1 4,8 ]hexad ecane 3 have been fully characterized by spectroscopic methods, including 2D NMR experiments, and satisfactory elemental analyses have been obtained. The structures of 2′ and 3 have been established unequivocally by single-crystal X-ray analyses (Figs. 1 and 2).‡ These compounds crystallise with two half ...