Coordination polymeric structures are of interest regarding crystal engineering with the aim to improve the design of extended structures [1]. When the synthesis involves the combination of two or more ligands into a mixed-ligand coordination polymer [2,3], it is still a great challenge to predict the composition and crystal structures.    Our intention was to build new coordination polymers starting from 3d metal salts (Zn2+, Ni2+), 4,4'bis((1H-imidazoyl-1-yl)methyl)-1,1'-biphenyl (BIMB) ligand and two polycarboxylic acids: 2,6pyridinedicarboxylic acid (2,6-H2PyDC) and 1,2,3-benzenetricarboxylic acid (1,2,3-H3BTC), respectively. The resulting compounds are: a dimer with molecular formula [Zn(BIMB)(2,6PyDC)] and a 2D polymer - {[Ni(BIMB)(1,3-BDC)(H2O)]·2H2O}n, where 1,3-BDC is the isophtalic acid obtained in situ during reaction (see the scheme below): Thermogravimetric analysis of the compounds was carried out in a nitrogen atmosphere up to 1000°C. Both compounds decompose in three stages and have a medium thermal stability. Ni compound loses water molecules from internal and external sphere of coordination until 390°C. After the first decomposition stage, a sudden loss of 40% (Ni) and 35% (Zn), and a gradual decomposition of the compounds occurs.   Although the crystal structure packaging for the two compounds show small cavities, the sorption properties are not very promising. The Ni and Zn compounds were tested towards N2 absorption at 77.3 K and the results for BET surface areas are 8.70 and 4.44 m2/g, and the pore volume is 0.028 and 0.015 ml/g, respectively. Unfortunately, these values are very low for practical applications.