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The metastable type‐II clathrate Na 24‐ δ  Ge 136  was obtained from Na 12 Ge 17  by applying a two‐step procedure. At first, Na 12 Ge 17  was reacted at 70 °C with a solution of benzophenone in the ionic liquid (IL) 1,3‐dibutyl‐2‐methylimidazolium‐bis(trifluoromethylsulfonyl) azanide. The IL was inert towards Na 12 Ge 17 , but capable of dissolving the sodium salts formed in the redox reaction. By annealing at 340 °C under an argon atmosphere, the X‐ray amorphous intermediate product was transformed to crystalline Na 24‐ δ  Ge 136  ( δ ≈2) and α‐Ge in an about 1 : 1 mass ratio. The product was characterized by X‐ray powder diffraction, chemical analysis, and  23 Na solid‐state NMR spectroscopy. Metallic properties of Na 24‐ δ  Ge 136  were revealed by a significant Knight shift of the  23 Na NMR signals and by a Pauli‐paramagnetic contribution to the magnetic susceptibility. At room temperature, Na 24‐ δ  Ge 136  slowly ages, with a tendency to volume decrease and sodium loss.

Type‐II Clathrate Na 24‐ δ Ge 136 from a Redox‐Preparation Route