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New metastable SmSi3−x (x=0–0.05) is obtained by high‐pressure high‐temperature synthesis (9.5 GPa, 870–1270 K). Powder diffraction data refinements reveal that the crystal structure of SmSi3 is isotypic to that of YbSi3 (space group I4/mmm, a=7.23634(5) Å, c=11.0854(1) Å). In the crystal structure, two types of Si2 dumbbells agglomerate into layers, which embed the samarium atoms. At ambient pressure,...