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Two coordinating compounds of zinc(II) (1) [Zn2(DAnH2)2(1,3-bdc)2(DMSO)4] and nickel(II) (2) [Ni(DAnH2)(1,4-bdc)(DMF)2]n were obtained based on dianilineglyoxime (DAnH2), 1,3-benzenedicarboxylic acid (1,3-bdcH2) and 1,4-benzenedicarboxylic acid (1,4-bdcH2), where DMSO is dimethylsulfoxide and DMF is dimethylformamide. The molecular and crystalline structure of reported compounds were established by infrared spectroscopy and single crystal X-ray diffraction, and for 1, additionally, the 1H and 13C NMR spectroscopy was used. According to data, the Zn(II) molecular complex is a binuclear and the Ni(II) is a 1D polymer compound.