Abstract
Solid-state reduction of WCl6 with Hg followed by incomplete sublimation of mercury chlorides generated the tritungsten decachloride—mercury chloride adducts W3Cl10(Hg2Cl2)2−x(HgCl2)x. Thermal equilibration of the solid-state products followed by sublimation of HgCl2 afforded single crystals that include the mercurous chloride adduct W3Cl10(Hg2Cl2)2. Single-crystal diffractometry revealed a one-dimensional polymer of tritungsten decachloride triangular clusters with novel terminal and inter-cluster-bridging ClHgHgCl ligands. The W3 cluster core has similar metrics to that of the benzyltriethylammonium salt of W3(μ3-Cl)(μ-Cl)3Cl9 3−. W3Cl10(Hg2Cl2)2 is the first reported adduct of the binary tungsten chloride W3Cl10. The ClHgHgCl ligands are more labile that the terminal chlorine atoms of W3(μ3-Cl)(μ-Cl)3Cl9 3−. These results demonstrate diverse roles and potential utility of main group element halide by-product ligands in solid-state reductions of transition metal halides.
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