Two new oxamido‐bridged N4 macrocyclic complexes [(CuL)2Mn(C2H5OH)2](ClO4)2·2C2H5OH (1) and [(CuL)2Co‐(C2H5OH)2](ClO4)2·2C2H5OH (2) (H2L = 2,3‐dioxo‐5,6:14,15‐di‐benzo‐7,13‐diphenyl‐1,4,8,12‐tetraazacyclo‐pentadeca‐7,13‐diene) have been synthesized and structurally characterized by X‐ray crystallographic investigations. In the two complexes, all copper(II) ions adopt a slightly distorted square‐planar configuration and the central manganese(II) and cobalt(II) ions are set in a distorted octahedral coordination sphere, connected to the other CuL fragments through exo‐cis oxamido bridges. The analyses of the magnetic properties were carried out by means of the theoretical expression of the magnetic susceptibility deduced from the spin Hamiltonian Ĥ = –2JŜ1Ŝ2, leading to J = –14.58 cm–1 for complex 1 and J = –26.95 cm–1 for complex 2, respectively.
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