Mononuclear macrocyclic complexes of manganese(II), cobalt(II) and nickel(II) perchlorate using 10 different oxaazamacrocyclic ligands (L1 — L10) have been prepared and characterized. The complexation reactions with the diiminic ligands were obtained by template condensation of the appropriate dialdehyde and diamine precursors; the reduced macrocycle complexes were synthesized using a direct route. The complexes have been characterized by elemental analyses, molar conductivity, mass spectrometry, IR, UV‐vis spectroscopy, diffuse reflectance and magnetic susceptibility measurements.