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Cs{sub 4}P{sub 2}Se{sub 10}: A new compound discovered with the application of solid-state and high temperature NMR

Abstract

The new compound Cs{sub 4}P{sub 2}Se{sub 10} was serendipitously produced in high purity during a high-temperature synthesis done in a nuclear magnetic resonance (NMR) spectrometer. {sup 31}P 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. Cs{sub 4}P{sub 2}Se{sub 10} has the triclinic space group P-1 with a=7.3587(11) A, b=7.4546(11) A, c=10.1420(15) A, {alpha}=85.938(2){sup o}, {beta}=88.055(2){sup o}, and {gamma}=85.609(2){sup o} and contains the [P{sub 2}Se{sub 10}]{sup 4-} anion. To our knowledge, this is the first compound containing this anion that is composed of two tetrahedral (PSe{sub 4}) units connected by a diselenide linkage. It was also possible to form a glass by quenching the melt in ice water, and Cs{sub 4}P{sub 2}Se{sub 10} was recovered upon annealing. The static {sup 31}P NMR spectrum at 350 deg. C contained a single peak with a -35 ppm chemical shift and a {approx}7 ppm peak width. This study highlights the potential of solid-state and high-temperature NMR for aiding  More>>
Publication Date:
Oct 15, 2007
Product Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 10; Other Information: DOI: 10.1016/j.jssc.2007.08.002; PII: S0022-4596(07)00314-3; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ANIONS; ANNEALING; CESIUM COMPOUNDS; CHEMICAL SHIFT; GLASS; MONOCRYSTALS; NMR SPECTRA; NMR SPECTROMETERS; NUCLEAR MAGNETIC RESONANCE; PHOSPHIDES; QUENCHING; SELENIDES; SPACE GROUPS; SYNTHESIS; TRICLINIC LATTICES; X-RAY DIFFRACTION
OSTI ID:
21049523
Country of Origin:
United States
Language:
English
Other Identifying Numbers:
Journal ID: ISSN 0022-4596; JSSCBI; TRN: US08R1024061656
Availability:
Available from http://dx.doi.org/10.1016/j.jssc.2007.08.002;INIS
Submitting Site:
INIS
Size:
page(s) 2877-2884
Announcement Date:
Aug 07, 2008

Citation Formats

Gave, Matthew A, Canlas, Christian G, Chung, In, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], Iyer, Ratnasabapathy G, Kanatzidis, Mercouri G, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], E-mail: m-kanatzidis@northwestern.edu, and Weliky, David P. , E-mail: weliky@chemistry.msu.edu. Cs{sub 4}P{sub 2}Se{sub 10}: A new compound discovered with the application of solid-state and high temperature NMR. United States: N. p., 2007. Web. doi:10.1016/j.jssc.2007.08.002.
Gave, Matthew A, Canlas, Christian G, Chung, In, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], Iyer, Ratnasabapathy G, Kanatzidis, Mercouri G, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], E-mail: m-kanatzidis@northwestern.edu, & Weliky, David P. , E-mail: weliky@chemistry.msu.edu. Cs{sub 4}P{sub 2}Se{sub 10}: A new compound discovered with the application of solid-state and high temperature NMR. United States. https://doi.org/10.1016/j.jssc.2007.08.002
Gave, Matthew A, Canlas, Christian G, Chung, In, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], Iyer, Ratnasabapathy G, Kanatzidis, Mercouri G, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], E-mail: m-kanatzidis@northwestern.edu, and Weliky, David P. , E-mail: weliky@chemistry.msu.edu. 2007. "Cs{sub 4}P{sub 2}Se{sub 10}: A new compound discovered with the application of solid-state and high temperature NMR." United States. https://doi.org/10.1016/j.jssc.2007.08.002.
@misc{etde_21049523,
title = {Cs{sub 4}P{sub 2}Se{sub 10}: A new compound discovered with the application of solid-state and high temperature NMR}
author = {Gave, Matthew A, Canlas, Christian G, Chung, In, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], Iyer, Ratnasabapathy G, Kanatzidis, Mercouri G, Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)], E-mail: m-kanatzidis@northwestern.edu, and Weliky, David P. , E-mail: weliky@chemistry.msu.edu}
abstractNote = {The new compound Cs{sub 4}P{sub 2}Se{sub 10} was serendipitously produced in high purity during a high-temperature synthesis done in a nuclear magnetic resonance (NMR) spectrometer. {sup 31}P 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. Cs{sub 4}P{sub 2}Se{sub 10} has the triclinic space group P-1 with a=7.3587(11) A, b=7.4546(11) A, c=10.1420(15) A, {alpha}=85.938(2){sup o}, {beta}=88.055(2){sup o}, and {gamma}=85.609(2){sup o} and contains the [P{sub 2}Se{sub 10}]{sup 4-} anion. To our knowledge, this is the first compound containing this anion that is composed of two tetrahedral (PSe{sub 4}) units connected by a diselenide linkage. It was also possible to form a glass by quenching the melt in ice water, and Cs{sub 4}P{sub 2}Se{sub 10} was recovered upon annealing. The static {sup 31}P NMR spectrum at 350 deg. C contained a single peak with a -35 ppm chemical shift and a {approx}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. - Graphical abstract: The new compound Cs{sub 4}P{sub 2}Se{sub 10} was discovered following a high-temperature in situ synthesis in the NMR spectrometer and the structure was determined by single-crystal X-ray diffraction. It contains the new [P{sub 2}Se{sub 10}]{sup 4-} anion.}
doi = {10.1016/j.jssc.2007.08.002}
journal = []
issue = {10}
volume = {180}
place = {United States}
year = {2007}
month = {Oct}
}