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Arsenic(III)-oxide Intercalates with Potassium Chloride: Water-Induced Varieties and New Synthesis Methods

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posted on 23.07.2021, 22:29 by Mateusz A. Domański, Karol Kraszewski, Piotr Paluch, Piotr A. Guńka
Synthesis and crystal structure determination of two new arsenic­(III)-oxide intercalates with potassium chloride, KCl·As2O3·1/2H2O and KCl·As2O3·3H2O, are reported, and the crystal structure of the anhydrous KCl·2As2O3 intercalate is redetermined. New ambient-pressure and ambient-temperature synthesis methods of the compounds are described including a mechanochemical route. Thermal stability of the compounds has been evaluated, and KCl·As2O3·3H2O was found to transform into KCl·As2O3·1/2H2O upon heating at 120 °C. Thermogravimetric measurements together with infrared and solid-state 1H nuclear magnetic resonance spectroscopy revealed the presence of water in KCl·As2O3·1/2H2O. The results of the structural studies on this compound have led to a proposal for corrections in the crystal structure model of the NH4Cl·As2O3·1/2H2O intercalate. Last but not least, interlayer interaction energies in KCl·2As2O3 have been calculated and compared to analogous energies in KN3·2As2O3, which revealed similarities in the energetic factors stabilizing both compounds.