Ag[WI] and A[WI] compounds with A = Na, Li were prepared from binary tungsten iodides (WI) and corresponding metal iodides. Their crystal structures are analyzed on the basis of X-ray diffraction data. Li andNa solid-state NMR measurements reveal that Li and Na ions are distributed over two sites in the respective structures. These results shed some new light on A [MI] with A = alkali and M = Mo, W compounds being reported with x = 1 and 2, which exhibit photophysical properties. The lithium compound is an exception in the series of A[WI] compounds, because it is the only compound which is soluble in water.
Alkaline earth tungsten iodide clusters AE[W6I14] with AE = Mg, Ca, Sr, Ba and the solvated compound [Ca(C2H6SO)6][W6I14] were prepared and structurally characterized. A new synthesis was employed, starting from W6I22, which is an exceptional compound among binary tungsten iodides because it is soluble in common polar organic solvents. As evidence for the wide range of the applicability of W6I22, we report the synthesis of the new AE[W6I14] compounds in comparison to a solid‐state reaction departing from W3I12.
The reduction of tungsten hexachloride with lead powder was investigated by differential scanning calorimetry (DSC) combined with X-ray diffraction (XRD) studies. Intermediate compounds along the way of the reduction of W to W were detected, prepared by solid-state synthesis, and structurally characterized by X-ray diffraction techniques. Five new compounds, namely PbWCl, PbWCl, Pb[WCl], PbCl[WCl], and Pb[WCl] are discovered to be formed with increasing temperature, and structurally characterized within this study. The analysis of the reduction pathway is meant to gain a better understanding of the metallothermic reduction process and intercalation chemistry in the solid state.
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