16-Membered benzoazo-and benzoazoxycrown ethers have been synthesized by reductive macrocyclization of respective bis (nitrophenoxy) oxaalkanes. The isomers of azocrown ethers were separated and E and Z structures were ascribed. Behavior of the compounds as ionophores in ion-selective membrane electrodes has been studied. Structure of Z isomer of 16-membered tribenzoazocrown ether has been determined.
