Abstract: | Two heterometallic trinuclear complexes of macrocyclic oxamide Co(Ni L1 )2 L2 (H2O)] · 3H2O ( 1 ) and Mn(Ni L1 )2 L2 (H2O)] · 0.5CH3OH · 1.5H2O ( 2 ) (H2 L1 = 2,3‐dioxo‐5,6,14,15‐dibenzo‐1,4,8,12‐tetraazacyclopentadeca‐7,13‐diene, H2 L2 = 5‐sulfosalicylic acid) were synthesized and structurally characterized by elemental analysis, IR spectroscopy, and X‐ray diffraction. Single‐crystal X‐ray analyses reveal that both the complexes contain discrete neutral trinuclear (Ni L1 )2M L2 (H2O)] (for 1 and 2 , M = Co, Mn, respectively) moieties. The structures of 1 and 2 have oxamido‐bridged trinuclear MIINiII2] units and consist of one‐dimensional chains formed by strong intermolecular hydrogen bonds. Furthermore, the magnetic properties of complex 1 were investigated and discussed in detail. |