Two coordination polymers (CPs), namely, [Zn(BPDC)(3bpdb) 0.5 (H 2 O) 2 ] n (1), and [Ni(BPDC)(3-bpdb)(H 2 O) 2 ] n (2) (where H 2 BPDC = 4,4'-biphenyldicarboxylic acid, 3-bpdb = 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene) have been solvothermally synthesized and characterized by single-crystal X-ray diffraction, IR, elemental analyses, PXRD, and SEM. CP 1 possesses a 2D 3-connected hcb net, and weak hydrogen bonding and π•••π stacking contacts further link the 2D networks to form 3D supramolecular structure. The structure