New metallomacrocyclic complexes based on acetamidrazone

The reaction of the linear polyether dialdehyde 3,3'-(3,6-dioxaoctane-1,8-d iyldioxy)-bis(2-hydroxybenzaldehyde) (1) with acetamidrazone hydrochloride in the presence of barium triflate, followed by addition of metal(II) aceta te, where metal(II) = nickel(II), copper(II) or zinc(II), yields dimeric he terometallic complexes [NiBaL(CF3SO3)(2)](2) (2), [CuBaL(CF3SO3)(2)](2) (4) and [ZnBaL(CF3SO3)(2)(CH3OH)](2) (6). where H2L = macrocyclic ligand. Remo val of Ba2+ from 2, 4 and 6 by using an aqueous solution of guanidinium sul fate affords NiL . 2H(2)O (3), CuL . 1.5H(2)O (5) and ZnL . 2H(2)O (7). The crystal structure of 2 has been determined by X-ray diffraction methods. T he X-ray diffraction powder patterns show that 4 is isostructural with 2. E lectronic, EI. MALDI/TOF and ESI mass. NMR and ESR spectra are reported. Th ermal degradation bf 3. 5 and 7 gives pure metal(II) oxides. (C) 2000 Elsev ier Science S.A. All rights reserved.