Nickel, copper, and zinc complexes with salicylidenehydrazone of iminodiacetic acid (H 4 L): Cu 2 L ⋅ 2Py ⋅ 2CH 3 OH and Cu 2 ML(CH 3 COO) 2 (M= Ni, Cu, Zn) were synthesized and studied by thermo gravimetric analysis and IR and ESR spectroscopy. The crystal structure of the complex Cu 2 ZnL(CH 3 COO) 2 ⋅ 4Py ⋅ CH 3 OH was studied by X ray diffraction: space group C2/c, a = 31.6974 (12) Å, b = 10.3023(4) Å, c = 16.4714(7) Å; β = 119.7460(10)°; Z = 4; 3513 reflections with I > 2σ(I); R = 0.0382, R w = 0.1010. The tem perature dependences of the ESR spectra of liquid solutions and the magnetic susceptibility of polycrystalline samples were studied. The ESR spectra of the binuclear copper complex and the trinuclear dicopper zinc complex exhibited hyperfine structure of seven lines, indicating exchange interaction of unpaired electrons with two equivalent copper nuclei.