To explore the influence of six structurally different polycarboxylate ligands H 2 L 1 to H 4 L 6 in the system Zn(II)/btmx, six coordination polymers, formulated as 5), and [Zn(btmx)-(H 2 L 6 )] n (6), have been obtained under similar conditions (btmx = 1,4-bis(1,2,4-triazol-1-ylmethyl)-2,3,5,6-tetramethylbenzene, H 2 L 1 = 1,3-benzenedicarboxylic acid, H 2 L 2 = 1,4benzenedicarboxylic acid, H 2 L 3 = 1,3-adamantanedicarboxylic acid, H 2 L 4 = 1,3-adamantanediacetic acid, H 2 L 5 = 4,4′oxidibenzoic acid, and H 4 L 6 = 3,3′,4,4′-benzophenone tetracarboxylic acid). The structure determination reveals that complexes 1 and 4 are two-dimensional (2D) layered networks and exhibit typical (4,4) topological nets. Complex 2 shows an undulating 2D (4,4)-network with 2-fold interpenetration. Complex 3 possesses a three-dimensional (3D) 3-fold interpenetrating 4-connected framework of 6 6 -dia topology. Both 5 and 6 have different 3D interpenetrated motifs generated by 2D → 3D interpenetration. Complex 5 belongs to a 3D framework built from the interpenetration of 2D bilayers in an inclined mode, while 6 involves a parallel interpenetration between the adjacent 2D (4,4) layers. This work markedly indicates that the effect of polycarboxylate ligands is significant in the construction of these networks.