By using a pre-designed anionic precursor [TpFeIII(CN)3]− (Tp = hydrotris(pyrazolyl)borate) as a structural building block, a new cyanide-bridged one-dimensional heterobimetallic coordination polymer, [(Tp)2Fe 2 III (CN)6Zn·2H2O] n (I) has been prepared and characterized by X-ray single crystal diffraction, Mossbauer and magnetic experiments. Complex I crystallizes in the orthorhombic Ibam space group with a = 14.4094(8) A, b = 18.3003(10) A, c = 12.9855(7) A and consists of rhombic chains, in which the [TpFeIII(CN)3]− unit acts as a bridging bidentate ligand toward two Zn2+ atoms through two of its three cyanide groups. [(Tp)2Fe 2 III (CN)6Zn·2H2O] n (I) crystallizes in the orthorhombic Ibam space group and consists of rhombic chains, in which the [TpFeIII(CN)3]− unit acts as a bridging bidentate ligand toward two Zn2+ atoms through two of its three cyanide groups.