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Three 1D/2D HgII coordination polymers (CPs), namely {[Hg3(L)2Cl6](H2O)}n (1), [Hg(L)Br2]n (2), and [Hg(L)I2]n (3) were prepared by assembly of 3,4‐bis(3‐pyridyl)‐5‐(4‐pyridyl)‐1,2,4‐triazole (L) with different inorganic HgII salts (i.e. HgCl2, HgBr2 or HgI2). Single‐crystal X‐ray diffraction analysis reveals two types of bimetallic subunits [(Hg)2C6N4] and [(Hg)2C12N6] in CP 1, which are further extended to a 2D coordination network. Both of CPs 2 and 3 show 1D zigzag arrays bridged by L ligands. Notably, the L ligands take the (η4, μ4) coordination fashion in 1 but (η2, μ2) binding mode in 2 and 3. The structural differences of CPs 1–3 indicate that the L ligand can adjust its coordination fashions to meet the requirements of HgII centers, relying on the presence of distinct halide anions. In addition, 1 can be applied to fabricate an electrochemical biosensor for the detection of penicillin. [ABSTRACT FROM AUTHOR]