Snap‐Shots of a Reduction Pathway: The Reaction of WCl₆ with Copper Powder

Abstract

A combined differential scanning calorimetry (DSC)/X‐ray diffraction (XRD) methodology is used to search and identify compounds in the Cu/W/Cl system based on the successive reaction of WCl6 with copper powder. Thermal effects monitored by DSC are used to detect reaction pathways and phase formations of compounds. A series of five new and one already known compounds is discovered as crystalline phases in the Cu/W/Cl system and structurally characterized by XRD. The reaction of WCl6 with elemental copper begins at temperatures as low as 60 °C with the formation of crystalline powders of α‐CuxWCl6. Continuing reaction stages include the successive formation of crystalline phases β‐CuxWCl6, γ‐CuxWCl6, α‐Cu2W2Cl10, β‐Cu2W2Cl10, and Cu2[W6Cl14].

Synthesis, Structure, and Electronic Properties of Sn9O5Cl4(CN2)2

“…The thermal scanning of chemical reactions can be a powerful method for the discovery of new compounds when compared to the classical explorative synthesis, where a mixture of solids is reacted at an intuitively selected temperature. The potential of the thermal scanning method has been demonstrated by the identification of more than 20 binary W–I compounds, by solid-state metathesis (SSM) reactions and by scanning a series of reduction reactions of WCl 6 to detect numerous compounds, for example, in the Pb–W–Cl, Co–W–Cl, Fe–W–Cl, and Cu–W–Cl systems. SSM reactions have been successfully employed for the development of metal compounds of nitridoborates, − cyanurates, and carbodiimides.…”