Nickel Decatungstate [Ni(C2H6SO)5(H2O)]2[W10O32]: Synthesis from a Water-Dimethylsulfoxide Solution, Crystal Structure Determination, IR and Raman Spectroscopic Analysis, Surface Micromorphology

Abstract

Crystalline nickel(II) decatungstate (II) [Ni(C₂H₆SO)₅(H₂O)]₂[W₁₀O₃₂] is synthesized for the first time and characterized by chemical and thermal analyses, scanning electron microscopy, IR and Raman spectroscopy, and single crystal X-ray diffraction (XRD). By single crystal XRD the crystallographic characteristics of [Ni(C₂H₆SO)₅(H₂O)]₂[W₁₀O₃₂] are determined (triclinic crystal system, space group P–1, a = 11.9339(7) Å, b = 12.2083(6) Å, c = 12.2083(6) Å, α = 75.235(5)°, β = 71.289(6)°, γ = 87.785(4)°, V = 1692.44(17) ų at T = 293(2) K, Z = 1, d_x = 3.223 g/cm³) and the structure is found to be composed of isolated [Ni(C₂H₆SO)₅(H₂O)]₂⁴⁺ cation complexes and [W₁₀O₃₂]^4– anions located in the voids between the cation complexes. By the powder XRD analysis it is shown that the crystals formed by growing from the solution do not contain impurities.