Abstract
The green crystals of Ni1.5H[Ni(OH)6W6O18]·12.5H2O and blue crystals of Na4[Ni(OH)6W6O18]·16H2O were isolated from the acidified (to Z = ν(H+)/ν(WO 2−4 ) = 1.00) solutions of Ni(NO3)2-Na2WO4-HNO3-H2O systems. The synthesized salts were identified by chemical analysis, XRPA, and IR spectroscopy. It was shown that the heteropolyanions belonged to the Anderson-Evans type of structure. An X-ray diffraction study of Na4[Ni(OH)6W6O18]·16H2O was carried out (M r = 1932.07, triclinic, space group P-1, a = 8.0089(11) Å, b = 10.5758(14) Å, c = 12.1987(16) Å; α = 69.268(13)°, β = 71.069(12)°, γ = 83.816(11)°; V = 914.0(2) Å3 at T = 293 K, Z = 1, ρcal = 3.510 g/cm3, F 000 = 874, μ = 19.470 mm−1, −16 ≤ h ≤ 16, −21 ≤ k ≤ 21, −24 ≤ l ≤ 24; the final R factors are R F = 0.0277, wR 2 = 0.0469 for the observed reflections (R F = 0.0606, wR 2 = 0.0523 for all independent reflections); S = 0.953; CSD-419883). The structure was solved by direct methods and refined in an anisotropic approximation. Hydrogen atoms were found in a difference synthesis and refined in an isotropic approximation with geometrical limitations. The nature of water in Na4[Ni(OH)6W6O18]·16H2O was characterized by DTA. XRPA was used to identify the thermolysis products of heteropoly compounds.
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Original Russian Text Copyright © 2009 by G. M. Rozantsev, S. V. Radio, N. I. Gumerova, V. N. Baumer, and O. B. Shishkin
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Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 311–319, March–April, 2009.
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Rozantsev, G.M., Radio, S.V., Gumerova, N.I. et al. Phase formation in the Ni2+-WO 2−4 -H+-H2O system (Z = 1.00). Crystal structure and properties of sodium heteropolyhexatunsten nickelate(2+) Na4[Ni(OH)6W6O18]·16H2O. J Struct Chem 50, 296–305 (2009). https://doi.org/10.1007/s10947-009-0041-z
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DOI: https://doi.org/10.1007/s10947-009-0041-z