CS4P2Se10: A new compound discovered with the application of solid-state and high temperature NMR

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The new compound CS4P2Se10 was serendipitously produced in high purity during a high-temperature synthesis done in a nuclear magnetic resonance (NMR) spectrometer. (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. Cs4P2Se10 has the triclinic space group P-1 with a = 7.3587(11)angstrom, b = 7.4546(11)angstrom, c = 10.1420(15)angstrom, alpha=85.938(2)degrees, beta=88.055(2)degrees, and gamma=85.609(2)degrees 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 P-31 NMR spectrum at 350 degrees C contained a single peak with a -35 ppm chemical shift and a similar to 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. (C) 2007 Elsevier Inc. All rights reserved.
Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
Issue Date
2007-10
Language
English
Article Type
Article
Keywords

METAL POLYSELENOPHOSPHATE FLUXES; SYSTEM PHOSPHORUS-SELENIUM; PHASE-CHANGE; SELENOPHOSPHATE COMPOUNDS; LOCAL-STRUCTURE; P-31; RB; EQUILIBRIA; KINETICS; SN2P2S6

Citation

JOURNAL OF SOLID STATE CHEMISTRY, v.180, no.10, pp.2877 - 2884

ISSN
0022-4596
DOI
10.1016/j.jssc.2007.08.002
URI
http://hdl.handle.net/10203/93216
Appears in Collection
NT-Journal Papers(저널논문)
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