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The hydrothermal reactions of molybdenum oxide starting materials with iron(II) and iron (III) halides in the presence of 2,2′-bipyridine have afforded the three related onedimensional solid materials [MoO 4 {Fe(III)Cl(2,2′-bpy)}] (1), [Mo 3 O 12 {Fe(III)(2,2′-bpy)} 2 ]‚0.25H 2 O (2), and [Mo 4 O 15 {Fe(III)(2,2′-bpy)} 2 ] (3). The structures of these three materials are based on a common one-dimensional ribbon exhibited by 1. The ribbon is constructed from fourpolyhedra rings consisting of two {MoO 4 } tetrahedra and two {FeXN 2 O 3 } (X ) Cl for 1, O for 2 and 3) octahedra. These polyhedra corner share such that each molybdenum center serves to bridge the two iron octahedra in the ring. Attachment to the next such four-ring is through the third corner sharing interaction of each molybdenum tetrahedron. Replacement of the pendant chloride substituents on adjacent iron centers in 1 with an {MoO 4 } unit leads to compound 2, while an {Mo 2 O 7 } linkage between adjacent iron centers affords 3.

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