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
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Gave, Matthew A;
Canlas, Christian G;
[1]
Chung, In;
[1]
Department of Chemistry, Northwestern University, Evanston, IL 60208 (United States)];
Iyer, Ratnasabapathy G;
[1]
Kanatzidis, Mercouri G;
[1]
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
[1]
- Department of Chemistry, Michigan State University, East Lansing, MI 48824 (United States)
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}
}
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}
}