The intercalation of Keggin-type [X(H2O)W11SiO39]6−(X=Co2+, Mn2+) heteropolyanions by aqueous anion exchange of 10 Å in a synthetic hydrotalcite-like Mg2Al(OH)6(NO3) results in products with interlayer spacing of ca. 10 Å. The layered array of the product and the integrity of the intercalated heteropolyanion are stable below 623 K in air as examined by XRD and IR analyses, respectively. UV-vis Diffuse Reflectance spectroscopy indicates that the water ligand in the intercalated [Co(H2O)W11SiO39]6− can be removed by thermal evacuation at 473 K leaving a coordinatively unsaturated site (in the transition metal) which reversibly coordinates water,methanol, ethanol or ammonia. ESR analysis of the intercalated [Mn(H2O)W11SiO39]6− shows that the shape of a signal at g = 2.00, arising from six-coordinated Mn2+ strongly depends on adsorption-desorption of the water ligand.
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