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. |