Scandium Selenophosphates: Structure and Properties of K4Sc2(PSe4)2(P2Se6)

Jonathan C. Syrigos; Mercouri G. Kanatzidis

doi:10.1021/acs.inorgchem.6b00535

Scandium Selenophosphates: Structure and Properties of K₄Sc₂(PSe₄)₂(P₂Se₆)

Jonathan C. Syrigos, Mercouri G. Kanatzidis^*

^*Corresponding author for this work

Chemistry

Research output: Contribution to journal › Article › peer-review

5 Scopus citations

Abstract

The new compound K₄Sc₂P₄Se₁₄ was synthesized via the polychalcogenide flux method. It crystallizes in the space group C2/c, and the structure is composed of ¹/_∞[Sc₂P₄Se₁₄^4-] chains that are separated by K⁺ cations. The structural motif features two [PSe₄]^3- units and one [P₂Se₆]^4- unit bridging the Sc centers and has not been reported for any other compound. The ¹/_∞[Sc₂P₄Se₁₄^4-] chains pack in a crosshatched pattern perpendicular to the c axis of the crystal, forming channels for half of the K⁺ atoms while the other half occupy empty space between the chains. The orange-yellow crystals of K₄Sc₂P₄Se₁₄ are air-sensitive and gradually turn red over the course of a couple hours. The band gap of the phase is 2.25(2) eV, and Raman spectroscopy shows the symmetric stretches of the selenophosphate groups to be at 231 and 216 cm^-1 for the [PSe₄]^3- and [P₂Se₆]^4- units, respectively. Solid-state ³¹P MAS NMR of K₄Sc₂P₄Se₁₄ shows two prominent peaks at 11.31 and -23.07 ppm and one minor peak at -106.36 ppm, most likely due to degradation of the product or an unknown second phase.

Original language	English (US)
Pages (from-to)	4664-4668
Number of pages	5
Journal	Inorganic chemistry
Volume	55
Issue number	9
DOIs	https://doi.org/10.1021/acs.inorgchem.6b00535
State	Published - May 2 2016

Funding

Financial support from the National Science Foundation (Grant DMR- 1410169) and from the Nicholson Fellowship is gratefully acknowledged. The SEM/EDS work was performed in the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by the NSF-DMR, Keck Foundation, State of Illinois, and Northwestern University.

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

Access to Document

10.1021/acs.inorgchem.6b00535

Cite this

@article{602ebc29c68d42708bd5cb8ddabc87bf,

title = "Scandium Selenophosphates: Structure and Properties of K4Sc2(PSe4)2(P2Se6)",

abstract = "The new compound K4Sc2P4Se14 was synthesized via the polychalcogenide flux method. It crystallizes in the space group C2/c, and the structure is composed of 1/∞[Sc2P4Se144-] chains that are separated by K+ cations. The structural motif features two [PSe4]3- units and one [P2Se6]4- unit bridging the Sc centers and has not been reported for any other compound. The 1/∞[Sc2P4Se144-] chains pack in a crosshatched pattern perpendicular to the c axis of the crystal, forming channels for half of the K+ atoms while the other half occupy empty space between the chains. The orange-yellow crystals of K4Sc2P4Se14 are air-sensitive and gradually turn red over the course of a couple hours. The band gap of the phase is 2.25(2) eV, and Raman spectroscopy shows the symmetric stretches of the selenophosphate groups to be at 231 and 216 cm-1 for the [PSe4]3- and [P2Se6]4- units, respectively. Solid-state 31P MAS NMR of K4Sc2P4Se14 shows two prominent peaks at 11.31 and -23.07 ppm and one minor peak at -106.36 ppm, most likely due to degradation of the product or an unknown second phase.",

author = "Syrigos, {Jonathan C.} and Kanatzidis, {Mercouri G.}",

note = "Funding Information: Financial support from the National Science Foundation (Grant DMR- 1410169) and from the Nicholson Fellowship is gratefully acknowledged. The SEM/EDS work was performed in the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by the NSF-DMR, Keck Foundation, State of Illinois, and Northwestern University. Publisher Copyright: {\textcopyright} 2016 American Chemical Society.",

year = "2016",

month = may,

day = "2",

doi = "10.1021/acs.inorgchem.6b00535",

language = "English (US)",

volume = "55",

pages = "4664--4668",

journal = "Inorganic chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "9",

}

TY - JOUR

T1 - Scandium Selenophosphates

T2 - Structure and Properties of K4Sc2(PSe4)2(P2Se6)

AU - Syrigos, Jonathan C.

AU - Kanatzidis, Mercouri G.

N1 - Funding Information: Financial support from the National Science Foundation (Grant DMR- 1410169) and from the Nicholson Fellowship is gratefully acknowledged. The SEM/EDS work was performed in the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by the NSF-DMR, Keck Foundation, State of Illinois, and Northwestern University. Publisher Copyright: © 2016 American Chemical Society.

PY - 2016/5/2

Y1 - 2016/5/2

N2 - The new compound K4Sc2P4Se14 was synthesized via the polychalcogenide flux method. It crystallizes in the space group C2/c, and the structure is composed of 1/∞[Sc2P4Se144-] chains that are separated by K+ cations. The structural motif features two [PSe4]3- units and one [P2Se6]4- unit bridging the Sc centers and has not been reported for any other compound. The 1/∞[Sc2P4Se144-] chains pack in a crosshatched pattern perpendicular to the c axis of the crystal, forming channels for half of the K+ atoms while the other half occupy empty space between the chains. The orange-yellow crystals of K4Sc2P4Se14 are air-sensitive and gradually turn red over the course of a couple hours. The band gap of the phase is 2.25(2) eV, and Raman spectroscopy shows the symmetric stretches of the selenophosphate groups to be at 231 and 216 cm-1 for the [PSe4]3- and [P2Se6]4- units, respectively. Solid-state 31P MAS NMR of K4Sc2P4Se14 shows two prominent peaks at 11.31 and -23.07 ppm and one minor peak at -106.36 ppm, most likely due to degradation of the product or an unknown second phase.

AB - The new compound K4Sc2P4Se14 was synthesized via the polychalcogenide flux method. It crystallizes in the space group C2/c, and the structure is composed of 1/∞[Sc2P4Se144-] chains that are separated by K+ cations. The structural motif features two [PSe4]3- units and one [P2Se6]4- unit bridging the Sc centers and has not been reported for any other compound. The 1/∞[Sc2P4Se144-] chains pack in a crosshatched pattern perpendicular to the c axis of the crystal, forming channels for half of the K+ atoms while the other half occupy empty space between the chains. The orange-yellow crystals of K4Sc2P4Se14 are air-sensitive and gradually turn red over the course of a couple hours. The band gap of the phase is 2.25(2) eV, and Raman spectroscopy shows the symmetric stretches of the selenophosphate groups to be at 231 and 216 cm-1 for the [PSe4]3- and [P2Se6]4- units, respectively. Solid-state 31P MAS NMR of K4Sc2P4Se14 shows two prominent peaks at 11.31 and -23.07 ppm and one minor peak at -106.36 ppm, most likely due to degradation of the product or an unknown second phase.

UR - http://www.scopus.com/inward/record.url?scp=84968735499&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=84968735499&partnerID=8YFLogxK

U2 - 10.1021/acs.inorgchem.6b00535

DO - 10.1021/acs.inorgchem.6b00535

M3 - Article

C2 - 27078201

AN - SCOPUS:84968735499

SN - 0020-1669

VL - 55

SP - 4664

EP - 4668

JO - Inorganic chemistry

JF - Inorganic chemistry

IS - 9

ER -