High-pressure synthesis in diamond anvil cells can yield unique compounds with advanced properties, but often they are either unrecoverable at ambient conditions or produced in quantity insufficient for properties characterization. Here we report the synthesis of metallic, ultraincompressible ( K 0 = 428(10) GPa), and very hard (nanoindentation hardness 36.7(8) GPa) rhenium nitride pernitride Re 2 (N 2 )(N) 2 . Unlike known transition metals pernitrides Re 2 (N 2 )(N) 2 contains both pernitride N 2 4− and discrete N 3− anions, which explains its exceptional properties. Re 2 (N 2 )(N) 2 can be obtained via a reaction between rhenium and nitrogen in a diamond anvil cell at pressures from 40 to 90 GPa and is recoverable at ambient conditions. We develop a route to scale up its synthesis through a reaction between rhenium and ammonium azide, NH 4 N 3 , in a large-volume press at 33 GPa. Although metallic bonding is typically seen incompatible with intrinsic hardness, Re 2 (N 2 )(N) 2 turned to be at a threshold for superhard materials.

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Owing to intriguing materials properties non-metal nitrides are of special interest for both, solid-state chemistry and materials science. Mixed ternary non-metal nitrides, however, have only been sparsely investigated, as preparative chemistry lacks a systematic access, yet. Herein, we report on the highly condensed boron phosphorus nitride BP N , which was synthesized from (PNCl ) , NH N and h-BN in a high-pressure high-temperature reaction. By increasing partial pressure of HCl during synthesis using NH Cl, single-crystals of BP N up to 80 μm in length were obtained. The unprecedented framework-type structure determined by single-crystal XRD blends structural motifs of both, α-P N and c-BN, rendering BP N a double nitride. The compound was further investigated by Rietveld refinement, EDX, temperature-dependent PXRD, FTIR and solid-state NMR spectroscopy. The formation of BP N through use of reactive precursors exemplifies an innovative access to mixed non-metal nitrides.

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