Synthesis and Crystal Structure of Potassium-Nickel Heteropoly Hexatungstonickelate (II) K3Ni0,5[Ni(OH)(6)W6O18]center dot 12H(2)O with Anderson-Type Anion and Potassium-Nickel Paratungstate B K6Ni2[W12O40(OH)(2)]center dot 22H(2)O

摘要

Conditions necessary for the formation of potassium-nickel para-tungstate B K6Ni2[W12O40(OH)(2)]center dot 22H(2)O (1) and potassium-nickel heteropoly hexatungstonickelate (II) with Anderson type anion K3Ni0,5[Ni(OH)(6)W6O18]center dot 12H(2)O (2) in Ni(NO3)(2)-K2WO4-HNO3-H2O solution, acidified up to Z = nu(H+)/m(WO42-) = 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 (P) over bar, M-r = 3,628.59, a = 10.617(3) angstrom, b = 11.818(2) angstrom, c = 13.454(3) angstrom, alpha = 68.034(18)degrees, beta = 76.96(2)degrees, gamma = 63.53(2)degrees, V = 1,398.0(5); the compound 2 crystallizes in the monoclinic system, space group P2(1), M-r = 1,914.71, a = 11.2586(3) angstrom, b = 11.4933(6) angstrom, c = 26.1158(15) angstrom, alpha = 100.938(4)degrees, V = 3,318.0(3) angstrom(3). In the structure 1 paratungstate B anion [W12O40'(OH)(2)](10-) is centrosymmetric and occupies the center [[1/2,0,1/2]], while 2D layers consist of isopolyanion and potassium polyhedra KOn (n = 8, 10), forming the 3D structure through NiO6 octahedra. The structure 2 comprises Anderson type anions [Ni(OH)(6)W6O18](4-), cationic polyhedra NiO6, KO8 and uncoordinated H2O molecules.