Two CoII- and NiII-based coordination polymers were prepared using 2,5-bis(1H-1,2,4-triazol-1-yl)terephthalic acid and M(OAc)2·4H2O (M = Co and Ni). In the two complex structures, the central CoII and NiII ions adopt distorted octahedral geometries, which are bound by the bifunctional ligands to produce a two-dimensional network. Magnetic studies reveal that the complexes show antiferromagnetic interactions.