Abstract
Conditions are determined for the formation of sodium heteropolyhexamolybdenumnickelate(II) Na4[Ni(OH)6Mo6O18]•16H2O (I) in a Ni(NO3)2–Na2МоO4–HNO3–H2O solution acidified to Z = = ν(H+)/ν(МоO42−) = 1.00. Synthesized salt I is investigated by chemical analysis, single crystal XRD, powder XRD, thermal analysis, and IR spectroscopy. The heteropolyanion is shown to belong to the Anderson type. Compound I is analyzed by single crystal XRD (Mr = 1404.61, triclinic, space group \(P\bar 1\), a = 8.0586(4) A, b = 10.5445(6) A, c = 12.1374(5) A, α = 69.557(5)°, β = 70.604(4)°, γ = 84.123(4)°, V = 911.45(8) A3) to find that it is isostructural to Na4[Ni(OH)6Mo6O18]•16H2O. All metal atoms in the structure of I are in an octahedral environment: the coordination sphere of the Ni heteroatom consists of OH groups; that of Mo consists of O atoms and OH groups; Na atoms are linked to the heteropolyanion via the terminal O atoms of the polyanion and surrounded by water molecules. In the crystal packing, the [Ni(OH)6Mo6O18]4– anions lie in planes parallel to \((1\bar 10)\) and the polyanion layers alternate with those formed by the paired octahedra [Na2(μ-H2O)2(H2O)6(O)2] in the direction of the y axis.
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