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Syntheses were performed at room temperature using Ni(NO 3 ) 2 ·6H 2 O, cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane) and the precursors Li 8 [Nb 6 O 19 ]· ≈22H 2 O or Na 7 [HNb 6 O 19 ]·15H 2 O in a DMSO-H 2 O mixture. Yellow crystals of the new compound {[Ni(cyclam)] 2 H 4 Nb 6 O 19 }·12H 2 O could be obtained after one week applying the Li +  or Na +  salt as starting materials. The crystal structure is unique in polyoxoniobate (PONb) chemistry and displays two interpenetrating three-dimensional (3D) networks. The [Nb 6 O 19 ] 8–  anion is expanded by four Ni 2+  centered complexes via Ni–O bonds to terminal O 2−  anions of the hexaniobate anion. The 3D networks are generated by further Ni–O bond formation between neighboring [Nb 6 O 19 ] 8−  anions. The remaining void space is occupied by H 2 O molecules which form a water cluster.

Hexaniobate anions connected by [Ni(cyclam)] 2+ complexes yield two interpenetrating three-dimensional networks