A potentially 18 donor macrocyclic ligand bearing four acetohydrazide pendant arms has been used to synthesize nine new dinuclear metal complexes with Co(II), Ni(II), Cu(II), Zn(II) and Cd(II). All compounds have been characterized by elemental analysis, MALDI-TOF-MS and FAB spectrometry, and by IR, UV–Vis and NMR spectroscopy. The system is a very good candidate for in situ recognition effects by MALDI-TOF-MS spectrometry and absorption spectroscopy. The presence of four acetohydrazide groups in L allows the synthesis of new three-dimensional self-assembling ditopic supramolecular compounds.