Synthesis and Crystal Structure of Potassium-Nickel Heteropoly Hexatungstonickelate (II) KNi[Ni(OH)WO]·12HO with Anderson-Type Anion and Potassium-Nickel Paratungstate B KNi[WO(OH)]·22HO.

Conditions necessary for the formation of potassium-nickel paratungstate B KNi[WO(OH)]·22HO ( 1) and potassium-nickel heteropoly hexatungstonickelate (II) with Anderson type anion KNi[Ni(OH)WO]·12HO ( 2) in Ni(NO)-KWO-HNO-HO solution, acidified up to Z = ν(H)/ν(WO) = 1,00, were established. The synthesized salts 1 and 2 were examined using chemical analysis, X-ray single crystal analysis and FTIR spectroscopy. The compound 1 crystallizes in the triclinic system, space group $$ \bar{P} $$ , M = 3,628.59, a = 10.617(3) Å, b = 11.818(2) Å, c = 13.454(3) Å, α = 68.034(18)°, β = 76.96(2)°, γ = 63.53(2)°, V = 1,398.0(5); the compound 2 crystallizes in the monoclinic system, space group P2 /n, M = 1,914.71, a = 11.2586(3) Å, b = 11.4933(6) Å, c = 26.1158(15) Å, α = 100.938(4)°, V = 3,318.0(3) Å. In the structure 1 paratungstate B anion [WO(OH)] is centrosymmetric and occupies the center [[1/2,0,1/2]], while 2D layers consist of isopolyanion and potassium polyhedra KO (n = 8, 10), forming the 3D structure through NiO octahedra. The structure 2 comprises Anderson type anions [Ni(OH)WO], cationic polyhedra NiO, KO and uncoordinated HO molecules. [ABSTRACT FROM AUTHOR]