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High-pressure/high-temperature conditions of 5.5 GPa and 750°C applied to a powder of Li 2 SiF 6 led to a pressure-supported crystal growth of Li 2 SiF 6 maintaining single crystals of sufficient quality for a single-crystal structure determination. The compound crystallizes in the space group P321 (No. 150) with 3 formula units and the lattice parameters a = 8.219(2), c = 4.5580(9) Å, V = 266.65(8) Å 3 , R 1 = 0.0178, and wR 2 = 0.0391 (all data).This work verified the published powder diffraction data of Li 2 SiF 6 and the predicted space group. Additionally, powder-FT-IR and Raman-spectroscopic investigations on single-crystals of Li 2 SiF 6 were performed for the first time.