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Title: High-Pressure Synthesis of a Pentazolate Salt

Abstract

The pentazolates, the last all-nitrogen members of the azole series, have been notoriously elusive for the last hundred years despite enormous efforts to make these compounds in either gas or condensed phases. Here, we report a successful synthesis of a solid state compound consisting of isolated pentazolate anions N5–, which is achieved by compressing and laser heating cesium azide (CsN3) mixed with N2 cryogenic liquid in a diamond anvil cell. The experiment was guided by theory, which predicted the transformation of the mixture at high pressures to a new compound, cesium pentazolate salt (CsN5). Electron transfer from Cs atoms to N5 rings enables both aromaticity in the pentazolates as well as ionic bonding in the CsN5 crystal. This work provides critical insight into the role of extreme conditions in exploring unusual bonding routes that ultimately lead to the formation of novel high nitrogen content species.

Authors:
; ; ; ; ; ORCiD logo
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1342252
Resource Type:
Journal Article
Journal Name:
Chemistry of Materials
Additional Journal Information:
Journal Volume: 29; Journal Issue: 2; Journal ID: ISSN 0897-4756
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
ENGLISH
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Steele, Brad A., Stavrou, Elissaios, Crowhurst, Jonathan C., Zaug, Joseph M., Prakapenka, Vitali B., and Oleynik, Ivan I. High-Pressure Synthesis of a Pentazolate Salt. United States: N. p., 2017. Web. doi:10.1021/acs.chemmater.6b04538.
Steele, Brad A., Stavrou, Elissaios, Crowhurst, Jonathan C., Zaug, Joseph M., Prakapenka, Vitali B., & Oleynik, Ivan I. High-Pressure Synthesis of a Pentazolate Salt. United States. doi:10.1021/acs.chemmater.6b04538.
Steele, Brad A., Stavrou, Elissaios, Crowhurst, Jonathan C., Zaug, Joseph M., Prakapenka, Vitali B., and Oleynik, Ivan I. Tue . "High-Pressure Synthesis of a Pentazolate Salt". United States. doi:10.1021/acs.chemmater.6b04538.
@article{osti_1342252,
title = {High-Pressure Synthesis of a Pentazolate Salt},
author = {Steele, Brad A. and Stavrou, Elissaios and Crowhurst, Jonathan C. and Zaug, Joseph M. and Prakapenka, Vitali B. and Oleynik, Ivan I.},
abstractNote = {The pentazolates, the last all-nitrogen members of the azole series, have been notoriously elusive for the last hundred years despite enormous efforts to make these compounds in either gas or condensed phases. Here, we report a successful synthesis of a solid state compound consisting of isolated pentazolate anions N5–, which is achieved by compressing and laser heating cesium azide (CsN3) mixed with N2 cryogenic liquid in a diamond anvil cell. The experiment was guided by theory, which predicted the transformation of the mixture at high pressures to a new compound, cesium pentazolate salt (CsN5). Electron transfer from Cs atoms to N5 rings enables both aromaticity in the pentazolates as well as ionic bonding in the CsN5 crystal. This work provides critical insight into the role of extreme conditions in exploring unusual bonding routes that ultimately lead to the formation of novel high nitrogen content species.},
doi = {10.1021/acs.chemmater.6b04538},
journal = {Chemistry of Materials},
issn = {0897-4756},
number = 2,
volume = 29,
place = {United States},
year = {2017},
month = {1}
}

Works referencing / citing this record:

Stabilization of the Pentazolate Anion in Three Anhydrous and Metal-Free Energetic Salts
journal, March 2018

  • Xu, Yuangang; Lin, Qiuhan; Wang, Pengcheng
  • Chemistry - An Asian Journal, Vol. 13, Issue 8
  • DOI: 10.1002/asia.201800187

Syntheses, Crystal Structures and Properties of a Series of 3D Metal–Inorganic Frameworks Containing Pentazolate Anion
journal, May 2018

  • Xu, Yuangang; Lin, Qiuhan; Wang, Pengcheng
  • Chemistry – An Asian Journal, Vol. 13, Issue 13
  • DOI: 10.1002/asia.201800476

Self-assembled energetic coordination polymers based on multidentate pentazole cyclo-N5−
journal, April 2018


A series of energetic metal pentazolate hydrates
journal, August 2017


Self-assembled energetic 3D metal–organic framework [Na 8 (N 5 ) 8 (H 2 O) 3 ] n based on cyclo -N 5
journal, January 2018

  • Xu, Yuangang; Wang, Pengcheng; Lin, Qiuhan
  • Dalton Transactions, Vol. 47, Issue 5
  • DOI: 10.1039/c7dt04501h

Single-crystal diffractometer coupled with double-sided laser heating system at the Extreme Conditions Beamline P02.2 at PETRAIII
journal, July 2019

  • Bykova, Elena; Aprilis, Georgios; Bykov, Maxim
  • Review of Scientific Instruments, Vol. 90, Issue 7
  • DOI: 10.1063/1.5108881

Synthesis of FeN 4 at 180 GPa and its crystal structure from a submicron-sized grain
journal, September 2018

  • Bykov, Maxim; Khandarkhaeva, Saiana; Fedotenko, Timofey
  • Acta Crystallographica Section E Crystallographic Communications, Vol. 74, Issue 10
  • DOI: 10.1107/s2056989018012161