A series of dimeric complexes have been isolated by the reaction of M(CH3COO)2·xH2O (MII=Ni, Pb) with nitrilo-tris (methylenephenylphosphinic) acid (H3L) in dimethylsulfoxide or pyridine or water. A complete single crystal structure determination has been carried out on the nickel derivative, which displays a dimeric structure [Ni(HL)(DMSO)]2·2DMSO. All the
compounds have been characterized through magnetic measurements, thermogravimetric and calorimetric analyses.