Abstract Hydrothermal synthesis, crystal structure and properties of a new heterometallic coordination polymer [(VO(terpy))4(MoO4)2(Mo8O26)]·2H2O (1) (terpy = 2,2′;6′,2″-terpyridine) are reported. Compound 1 contains two crystallographically unique vanadium(IV) atoms, bonded to a terminal oxido ligand and further coordinated to a terpy ligand. The three N atoms of terpy occupy the meridional sites of a distorted {VN3O3} octahedron. A γ-octamolybdate (Mo8O26)4– located on an inversion centre and a tetraoxidomolybdate (MoO4)2– function as bridging ligands. The μ3-bridging tridentate binding of (MoO4)2– leads to the formation of a {V4Mo2O12}4+ cationic unit consisting of an eight-membered heterometallic {Mo2V2O4} ring with protruding oxidovanadium handles. A pair of {V4Mo2O12}4+ units are bridged by the centrosymmetric (Mo8O26)4– ligand, resulting in the formation of an infinite chain of alternating {V4Mo2O12}4+ cations and (Mo8O26)4– anions.
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