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 journalArticle

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 2007

Fingerprint

Nuclear magnetic resonance
solid state
nuclear magnetic resonance
Chemical shift
Anions
chemical equilibrium
Negative ions
Magnetic resonance spectrometers
Temperature
temperature
anions
Magic angle spinning
ampoules
Ice
synthesis
products
linkages
Phosphorus
metal spinning
phosphorus

Keywords

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

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

Cs4P2Se10 : A new compound discovered with the application of solid-state and high temperature NMR. / Gave, Matthew A.; Canlas, Christian G.; Chung, In; Iyer, Ratnasabapathy G.; Kanatzidis, Mercouri G; Weliky, David P.

In: Journal of Solid State Chemistry, Vol. 180, No. 10, 10.2007, p. 2877-2884.

Research output: Contribution to journalArticle

Gave, Matthew A. ; Canlas, Christian G. ; Chung, In ; Iyer, Ratnasabapathy G. ; Kanatzidis, Mercouri G ; Weliky, David P. / Cs4P2Se10 : A new compound discovered with the application of solid-state and high temperature NMR. In: Journal of Solid State Chemistry. 2007 ; Vol. 180, No. 10. pp. 2877-2884.
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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) {\AA}, b=7.4546(11) {\AA}, c=10.1420(15) {\AA}, 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.",
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AB - 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.

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