Abstract: Four dimeric and polymeric coordination compounds [Zn2(bimb)2(pdc)2]·6H2O (1), [Cd2(bimb)2(tp)2]·H2O (2), [Cd(bimb)(ada)] (3) and [Co(bimb)(ada)] (4) (bimb, 4,4′-bis(imidazol-1-ylmethyl)biphenyl; pdc, pyridine-2,6-dicarboxylate; tp, terephthalate and ada, adipate) have been synthesized under hydrothermal conditions. Complex 1 is a discrete dinuclear metallomacrocycle featuring a 34-membered ring, in which the flexible bimb ligand acts as syn-conformation. While complexes 2–4 are 3D network structures connected by bimb and dicarboxylate ligands, the bimb ligand displays anti-confromation. [Copyright &y& Elsevier]