Cs4P2Se10: A new compound discovered with the application of solid-state and high temperature NMR

Matthew A. Gave, Christian G. Canlas, In Chung, Ratnasabapathy G. Iyer, Mercouri G. Kanatzidis, David P. Weliky

Research output: Contribution to journalArticlepeer-review

7 Citations (Scopus)

Abstract

The new compound Cs4P2Se10 was serendipitously produced in high purity during a high-temperature synthesis done in a nuclear magnetic resonance (NMR) spectrometer. 31P magic angle spinning (MAS) NMR of the products of the synthesis revealed that the dominant phosphorus-containing product had a chemical shift of -52.8 ppm that could not be assigned to any known compound. Deep reddish brown well-formed plate-like crystals were isolated from the NMR reaction ampoule and the structure was solved with X-ray diffraction. Cs4P2Se10 has the triclinic space group P-1 with a=7.3587(11) Å, b=7.4546(11) Å, c=10.1420(15) Å, α=85.938(2)°, β=88.055(2)°, and γ=85.609(2)° and contains the [P2Se10]4- anion. To our knowledge, this is the first compound containing this anion that is composed of two tetrahedral (PSe4) units connected by a diselenide linkage. It was also possible to form a glass by quenching the melt in ice water, and Cs4P2Se10 was recovered upon annealing. The static 31P NMR spectrum at 350 °C contained a single peak with a -35 ppm chemical shift and a ∼7 ppm peak width. This study highlights the potential of solid-state and high-temperature NMR for aiding discovery of new compounds and for probing the species that exist at high temperature.

Original languageEnglish
Pages (from-to)2877-2884
Number of pages8
JournalJournal of Solid State Chemistry
Volume180
Issue number10
DOIs
Publication statusPublished - Oct 1 2007

Keywords

  • Chalcogenides
  • High temperature
  • Metal selenophosphates
  • NMR
  • P
  • Phosphorus
  • Solid state

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Ceramics and Composites
  • Condensed Matter Physics
  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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