The complexes of transition metals with dioxime ligands occupy an important place in the coordination chemistry [1]. Also described are compounds of the dioximes in which the evolution from low nuclearity compounds to polynuclear [2]. Dianilineglyloxime is a monofunctional ligand, which does not allow the creation of polynuclear complexes, therefore it is necessary to include bridge-function ligands. In this way, the 1D polymer of Ni(II) with DAnH2 and terephthalic acid (1,4-H2bdc) was synthesized according to the scheme below, at a molar ratio of 1: 2: 2. Ni(CH3COO)2·4H2O + 2DAnH2 + 2(1,4-H2bdc) → [Ni(DAnH2)(1,4-bdc)(DMF)2]n The structure and composition of the complex were determined by combined thermogravimetric analysis (TG, DTG and DTA) in the 20-1000°C range in air, with a heating rate of 10°C/min. (Figure 1), X-ray diffraction, IR and NMR spectroscopy. Up to 244oC there is a 25% mass loss that corresponds to the two coordinated DMF molecules. Another 14% loss occurs up to 332°C, where two CO2 molecules from the acid are lost, while the aromatic fragment decomposes up to 416°C with a loss of 14.12%. At 536°C, the total decomposition of the polymer takes place with the formation of a NiO residue.figureFigure 1. TG/DTG/DTA patterns of Ni(II) 2D polymer.