The copper(II) and nickel(II) complexes based on bis(azomethine), which is the condensation product of 1-phenyl-3-methyl-4-formyl-5-mercaptopyrazole with 1,3-diaminopropan-2-ol, are synthesized. Bis-azomethines can form both binuclear and mononuclear complexes in which the hydroxy group is not involved in coordination. The binuclear copper(II) complexes with the acetate and pyrazolate bridges exhibit an antiferromagnetic exchange, which strength is determined by the nature of the bridge (2J = −154 and −424 cm−1, respectively). The structure parameters of the coordination spheres of the complexes are determined by X-ray absorption spectroscopy. The structure of the CHCl3 solvate of the binuclear copper(II) complex with the pyrazolate bridge is solved by X-ray diffraction analysis (CIF file CCDC 964655).