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A new bicapped Keggin heteropolyoxoanion derivative [Co(bpy) 3 ] 2 [V IV O 40 (V IV O) 2 ] [{Co(bpy) 2 (H 2 O)} 2 {V IV O 40 (V IV O) 2 }]  ·  8H 2 O (1) (bpy  =  2,2′-bipyridine), has been hydrothermally synthesized and structurally characterized by elemental analysis, single crystal X-ray diffraction, IR and X-ray photoelectron spectra. Complex 1 consists of two [Co(bpy) 3 ] 2+ cations, an anion of [V IV O 40 (V IV O) 2 ] 4- and a neutral unit [{Co(bpy) 2 (H 2 O)} 2 {V IV O 40 (V IV O) 2 }] in which {V IV O 40 (V IV O) 2 } 4- is coordinated to two Co atoms through its terminal oxygen atoms of the two capping V atoms at opposite sites together with bipyridine and water ligands. The most interesting feature of 1 is that a polyoxoanion and a neutral component coexist in the crystal structure. Hydrogen-bonding contacts are also formed between different polyanions through the lattice water molecules. [ABSTRACT FROM AUTHOR]