The self-assembly of [Zn(L)(H 2 O) 2 ]·Cl 2 and 1,2-cyclopentanedicarboxylic acid generates a 2D hydrogen-bonded polymer [Zn(L)(Hcpdc)] (L = 3,14-dimethyl -2,6,13,17-tetraazatricyclo[14,4,0 1.18 0 7.12 ]docosane, H 2 cpdc= 1,2-cyclopentanedicarboxylic acid) (1). Complex 1 is characterized by X-ray crystallography, spectroscopy, and thermogravimetric analyzer. The crystal structure of 1 shows a distorted octahedral coordination geometry around the zinc (II) ion, with the four secondary amines of the macrocycle and two carboxylate oxygen atoms of the Hcpdc -ligand in the trans position. The compound crystallizes in the monoclinic system P2 1 /c with a = 8.6002(10), b = 10.4906(11), c = 19.008(2) Å, β (°) = 92.949(7)°, V = 1712.6(3) Å 3 , Z = 2. The IR spectrum and TGA behavior of the compound are significantly affected by the Hcpdc -ligand.