Potassium hexahydroperoxostannate: synthesis and structure. Ippolitov E.G., Tripol'skaya T.A., Prikhodchenko P.V., Pankratov D.A. //Russian Journal of Inorganic Chemistry. 2001. V.46. №6. P.851-857
Polycrystalline potassium hexahydroperoxostannate was prepared by replacement of hydroxo groups in potassium hexahydroxostannate upon its dissolution in hydrogen peroxide. A comparative study of the product and the starting hydroxostannate by powder X-ray diffraction analysis, thermogravimetry, and IR, 2H, 39K, and 119Sn NMR, and Mössbauer spectroscopy was carried out. The peroxo compound K2Sn(OOH)6 crystallizes in the hexagonal system with a = 7.264(7) Å, c = 10.168(4) Å. IR, NMR, and Mössbauer spectroscopy data show that the tin coordination polyhedron in the peroxo compound is an octahedron formed by the coordinated hydroperoxo groups.
Previously, sodium hexahydroperoxostannate was prepared and characterized by powder X-ray diffraction analysis, thermogravimetry, IR, 1H NMR, and Mossbauer spectroscopy, and by thermodynamic and kinetic method. The tin atom in this compound were found to occur in the octahedral environment of hydroperoxo group. It appeared pertinent to confirm the possibility of formation of this type of tin compound by preparing a new hydroperoxo complex. To this end, we performed the first synthesis of potassium hexahydroperoxostannate. Comparative study of potassium hexahydrosstannate (1) and hexahydroperoxosstannate (2) and their deuterated analogue (1a and 2a, respectively) was carried out by powder X-ray diffraction analysis, thermogravimetry, and IR, NMR (2H, 39K and 119Sn), and Mossbauer spectroscopy.