Abstract: Complexes CuL1 ⋅ MeOH (Ia), NiL1 ⋅ MeOH (Ib), CоL1 ⋅ MeOH (Ic), CuL2 (IIa), NiL2 (IIb), and CоL2 (IIc) of the tetradentate azomethine compounds, namely, 4-methyl-N-[2-[(E)-2-[2-[2-[(E)-[2-(p-toluenesulfamino)phenyl]methyleneamino]ethoxy]ethyliminomethyl]phenyl]benzenesulfamide (H2L1) and 4-methyl-N-[2-[(E)-3-[4-[3-[(E)-[2-(p-toluenesulfamino)phenyl]methyleneamino]propoxy]butoxy]-propyliminomethyl]phenyl]benzenesulfamide (H2L2), which are the condensation products of 2-(N-tosylamino)benzaldehyde with 3,4-dioxa-1,8-octanediamine and 4,9-dioxa-1,12-dodecanediamine, are synthesized using the chemical and electrochemical methods. The structures, compositions, and properties of the synthesized metal complexes are studied by the methods of elemental analysis, IR spectroscopy, X-ray absorption spectroscopy, magnetochemistry, and X-ray diffraction analysis (СIF files CCDC nos. 1910746 (Ia), 1910747 (Ib), and 1910748 (Ic)). In the molecules of compounds Ia–Ic, the L1 macrocyclic ligand coordinates the metal atom by four nitrogen atoms via the tetradentate chelate mode to form the polyhedron as a distorted tetrahedron. © 2019, Pleiades Publishing, Ltd.