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Journal of Structural Chemistry

2011 year, number 1

CRYSTAL STRUCTURE OF NICKEL PARATUNGSTATE B Ni5[W12O40(ОН)2]·37H2O

S. V. Radio1, G. M. Rozantsev2, V. N. Baumer3, O. V. Shishkin4
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2
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4
Keywords: isopolytungstate, paratungstate B, crystal structure, FTIR spectroscopy, single crystal X-ray analysis
Pages: 115-121

Abstract

From the solution of the system Na2WO4-HNO3-Ni(NO3)2-H2O acidified to Z = ν(H+)/ν(WO) = 1.29, the green crystals of nickel paratungstate B Ni5[W12O40(ОН)2]·37H2O are isolated. By FTIR spectroscopy the isopoly anion is shown to belong to the structural type of paratungstate B. Using single crystal X-ray analysis, the structure of Ni5[W12O40(ОН)2]·37H2O is solved (Mr = 3840.36, monoclinic, P21/c space group, a = 21.9061(6) Å, b = 14.9297(4) Å, c = 22.1391(6) Å, β = 107.609(3)°, V = 6901.4(3) Å3 at T = 293 K, Z = 4, dx = 3.696 g/cm3, F000 = 6944, μ = 21.368 mm-1, -33 ≤ h ≤ 33, -22 ≤ k ≤ 22, -33 ≤ l ≤33; the final uncertainty values for the observed reflections are RF = 0.0532, wR2 = 0.0831 (RF = 0.1088, wR2 = 0.0894 over all independent reflections), S = 0.978; CSD-421468).