Synthesis of FeN<sub>4</sub>at 180 GPa and its crystal structure from a submicron-sized grain

Bykov, Maxim; Khandarkhaeva, Saiana; Fedotenko, Timofey; Sedmák, Pavel; Dubrovinsky, Leonid

doi:10.1107/s2056989018012161

Cited by 31 publications

(36 citation statements)

References 23 publications

(22 reference statements)

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“…The crystal structures are then solved and refined within the JANA2006 software 32 . The procedure for single crystal X-ray diffraction data acquisition and analysis was previously demonstrated and successfully employed 13,14,33,34 . Powder X-ray diffraction was also performed to verify the chemical homogeneity of the samples.…”

Section: Methodsmentioning

confidence: 99%

Synthesis of magnesium-nitrogen salts of polynitrogen anions

et al. 2019

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The synthesis of polynitrogen compounds is of fundamental importance due to their potential as environmentally-friendly high energy density materials. Attesting to the intrinsic difficulties related to their formation, only three polynitrogen ions, bulk stabilized as salts, are known. Here, magnesium and molecular nitrogen are compressed to about 50 GPa and laser-heated, producing two chemically simple salts of polynitrogen anions, MgN4 and Mg2N4. Single-crystal X-ray diffraction reveals infinite anionic polythiazyl-like 1D N-N chains in the crystal structure of MgN4 and cis-tetranitrogen N44− units in the two isosymmetric polymorphs of Mg2N4. The cis-tetranitrogen units are found to be recoverable at atmospheric pressure. Our results respond to the quest for polynitrogen entities stable at ambient conditions, reveal the potential of employing high pressures in their synthesis and enrich the nitrogen chemistry through the discovery of other nitrogen species, which provides further possibilities to design improved polynitrogen arrangements.

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Section: Methodsmentioning

confidence: 99%

Synthesis of magnesium-nitrogen salts of polynitrogen anions

et al. 2019

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“…Synthesis of such dinitrides requires very high pressure above 40–50 GPa and a simple synthetic route, which was actively exploited in the recent years, is a direct reaction between a metal and nitrogen in a laser‐heated diamond anvil cell (LHDAC). This method was successfully used for the synthesis of transition metal dinitrides (PtN 2 , PdN 2 , IrN 2 , OsN 2 , TiN 2 , RhN 2 , RuN 2 , CoN 2 , CuN 2 , FeN 2 , CrN 2 ), polynitrides (FeN 4 ,, ReN 8 · N 2 ), and alkali metal pentazolates (LiN 5 , CsN 5 ). To scale up the production the synthesis should be carried out in a large‐volume apparatus.…”

Section: Introductionmentioning

confidence: 99%

Synthesis of Arsenopyrite‐Type Rhodium Pernitride RhN₂ from a Single‐Source Azide Precursor

Bykov¹,

Yusenko

Bykova

et al. 2019

Eur J Inorg Chem

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Nitrogen‐rich noble metal nitrides possess unique mechanical and catalytic properties, therefore their synthesis and characterization is of interest for fundamental solid state chemistry and materials science. In this study we have synthesized a novel single‐source precursor [Rh(NH3)6]3(N3)5Cl4 (Rh/N ratio 1:11). Its controlled decomposition in a laser‐heated diamond anvil cell at 39 GPa resulted in a formation of rhodium pernitride RhN2. According to the results of single‐crystal X‐ray diffraction RhN2 has arsenopyrite structure type previously unknown for this compound [P21/c (no. 14), a = 4.694(3), b = 4.7100(6), c = 4.7198(7) Å, β =109.83(3) ° at 39 GPa].

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“…Recent high‐pressure studies have shown that various polynitrogen species may occur as a result of simple reaction between a metal and molecular nitrogen. Good examples of that are FeN 4 containing catena‐poly[tetraz‐1‐ene‐1,4‐diyl] anions [−N=N−N−N−] 2− ∞ , MgN 4 , and ReN 8 ⋅N 2 with polydiazenediyl (polyacetylene‐like) nitrogen chains . Thus, high‐pressure synthesis conditions enable the exploration of numerous possible metal–nitrogen framework topologies.…”

Section: Figurementioning

confidence: 99%

High‐Pressure Synthesis of Metal–Inorganic Frameworks Hf₄N₂₀⋅N₂, WN₈⋅N₂, and Os₅N₂₈⋅3 N₂ with Polymeric Nitrogen Linkers

et al. 2020

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Polynitrides are intrinsically thermodynamically unstable at ambient conditions and require peculiar synthetic approaches. Now, a one‐step synthesis of metal–inorganic frameworks Hf4N20⋅N2, WN8⋅N2, and Os5N28⋅3 N2 via direct reactions between elements in a diamond anvil cell at pressures exceeding 100 GPa is reported. The porous frameworks (Hf4N20, WN8, and Os5N28) are built from transition‐metal atoms linked either by polymeric polydiazenediyl (polyacetylene‐like) nitrogen chains or through dinitrogen units. Triply bound dinitrogen molecules occupy channels of these frameworks. Owing to conjugated polydiazenediyl chains, these compounds exhibit metallic properties. The high‐pressure reaction between Hf and N2 also leads to a non‐centrosymmetric polynitride Hf2N11 that features double‐helix catena‐poly[tetraz‐1‐ene‐1,4‐diyl] nitrogen chains [−N−N−N=N−]∞.

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Synthesis of FeN₄at 180 GPa and its crystal structure from a submicron-sized grain

Abstract: The refined crystal structure model of iron tetranitride, FeN4, at 180 GPa is similar to that at 135 GPa but shows improved structural parameters in terms of bond lengths and angles.

Cited by 31 publications

References 23 publications

Synthesis of magnesium-nitrogen salts of polynitrogen anions

Synthesis of magnesium-nitrogen salts of polynitrogen anions

Synthesis of Arsenopyrite‐Type Rhodium Pernitride RhN₂ from a Single‐Source Azide Precursor

High‐Pressure Synthesis of Metal–Inorganic Frameworks Hf₄N₂₀⋅N₂, WN₈⋅N₂, and Os₅N₂₈⋅3 N₂ with Polymeric Nitrogen Linkers

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Synthesis of FeN4at 180 GPa and its crystal structure from a submicron-sized grain

Abstract: The refined crystal structure model of iron tetra­nitride, FeN4, at 180 GPa is similar to that at 135 GPa but shows improved structural parameters in terms of bond lengths and angles.

Cited by 31 publications

References 23 publications

Synthesis of magnesium-nitrogen salts of polynitrogen anions

Synthesis of magnesium-nitrogen salts of polynitrogen anions

Synthesis of Arsenopyrite‐Type Rhodium Pernitride RhN2 from a Single‐Source Azide Precursor

High‐Pressure Synthesis of Metal–Inorganic Frameworks Hf4N20⋅N2, WN8⋅N2, and Os5N28⋅3 N2 with Polymeric Nitrogen Linkers

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Synthesis of FeN₄at 180 GPa and its crystal structure from a submicron-sized grain

Abstract: The refined crystal structure model of iron tetranitride, FeN4, at 180 GPa is similar to that at 135 GPa but shows improved structural parameters in terms of bond lengths and angles.

Synthesis of Arsenopyrite‐Type Rhodium Pernitride RhN₂ from a Single‐Source Azide Precursor

High‐Pressure Synthesis of Metal–Inorganic Frameworks Hf₄N₂₀⋅N₂, WN₈⋅N₂, and Os₅N₂₈⋅3 N₂ with Polymeric Nitrogen Linkers