Evidences of the non-stoichiometry and control of the composition of the cluster-based solid solution K6[Re6-xMoxS8(CN)5] (x=2.75-3.63) - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Journal of Solid State Chemistry Année : 2023

Evidences of the non-stoichiometry and control of the composition of the cluster-based solid solution K6[Re6-xMoxS8(CN)5] (x=2.75-3.63)

Résumé

In this work, we investigated a high-temperature reaction between ReS2, MoS2 and KCN resulting in the formation of the cluster-based K6[Re6-xMoxS8(CN)5] solid solution. The crystal structure is based on chains of [Re6-xMoxS8(CN)6] cluster units. It was found that both the sintering temperature of starting sulfides and the reaction temperature with KCN have an influence on the composition of the product allowing x to be varied within the range x = 2.75-3.63. The molar ration of ReS2:MoS2:KCN loaded composition is fixed to 3:3:14 in all experiments. Energy dispersive spectroscopy (EDS), powder X-ray diffraction (PXRD) and high-resolution electrospray (ESI) mass spectrometry were used to characterize the solid solution K6[Re6-xMoxS8(CN)5]. It was shown by mass spectrometry that the solid solution with fractional x contains anions based on the {Re4Mo2S8}, {Re3Mo3S8} and {Re2Mo4S8} cluster cores in different proportions depending on the above-mentioned factors. Particularly, the rise of the temperature of the synthesis or temperature of sintering of metal sulfides led to increase of the rhenium content in the solid solution.
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hal-03966567 , version 1 (31-01-2023)

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Tatiana Lappi, Yakov Gaifulin, Vadim Yanshole, Stephane Cordier, Nikolay Naumov. Evidences of the non-stoichiometry and control of the composition of the cluster-based solid solution K6[Re6-xMoxS8(CN)5] (x=2.75-3.63). Journal of Solid State Chemistry, 2023, 319, pp.123785. ⟨10.1016/j.jssc.2022.123785⟩. ⟨hal-03966567⟩
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