A convergent "5 + 1" and "5 + 3" synthetic strategy allowed the synthesis o
f the first examples of bis-betaines 2 and 3, a prototype of phanes that in
corporate heterocyclic betaines. The structure of the quadrupolar macrocycl
ic systems 2 and 3 together with the dicationic [1(6)]- and [1(8)] metahete
rophane precursors 5(.)2X and 6(.)2X were examined by spectroscopy using H-
1 and C-13 NMR techniques together with H-1-DNMR studies and electrospray i
onization mass spectrometry.