Structural studies of pendant diazacoronands having an N-benzoyl, N-acetyl, O-benzyl or O- benzoyl side arm were performed by means of X-ray and temperature-dependent 1H NMR experiments. The energies of macroring flipping process were determined for three pendant diazacoronands. The complexation properties of pendant diazacoronands toward the alkali metal cations (Na+, K+, and Rb+) were estimated by ESI-MS experiments.
