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Cr 5.7 Si 2.3 P 8 N 24 —A Chromium(+IV) Nitridosilicate Phosphate with Amphibole‐Type Structure

The first nitridic analog of an amphibole mineral, the quaternary nitridosilicate phosphate Cr 5.7 Si 2.3 P 8 N 24 was synthesized under high‐pressure high‐temperature conditions at 1400 °C and 12 GPa from the binary nitrides Cr 2 N, Si 3 N 4 and P 3 N 5 , using NH 4 N 3 and NH 4 F as additional nit...

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Bibliographic Details
Published in:Angewandte Chemie International Edition 2024-04, Vol.63 (14)
Main Authors: Pointner, Monika M., Fisher, Katherine R., Weidemann, Martin, Wolf, Florian, Wright, Jonathan P., Bright, Eleanor Lawrence, Giacobbe, Carlotta, Oeckler, Oliver, Schnick, Wolfgang
Format: Article
Language:English
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Summary:The first nitridic analog of an amphibole mineral, the quaternary nitridosilicate phosphate Cr 5.7 Si 2.3 P 8 N 24 was synthesized under high‐pressure high‐temperature conditions at 1400 °C and 12 GPa from the binary nitrides Cr 2 N, Si 3 N 4 and P 3 N 5 , using NH 4 N 3 and NH 4 F as additional nitrogen source and mineralizing agent, respectively. The crystal structure was elucidated by single‐crystal X‐ray diffraction with microfocused synchrotron radiation ( C 2/ m, a =9.6002(19), b =17.107(3), c =4.8530(10) Å, β= 109.65(3)°). The elemental composition was analyzed by energy dispersive X‐ray spectroscopy. The structure consists of vertex‐sharing PN 4 ‐tetrahedra forming zweier double chains and edge‐sharing (Si,Cr)‐centered octahedra forming separated ribbons. Atomic resolution scanning transmission electron microscopy shows ordered Si and Cr sites next to a disordered Si/Cr site. Optical spectroscopy indicates a band gap of 2.1 eV. Susceptibility measurements show paramagnetic behavior and support the oxidation state Cr +IV , which is confirmed by EPR. The comprehensive analysis expands the field of Cr−N chemistry and provides access to a nitride analog of one of the most prevalent silicate structures.
ISSN:1433-7851
1521-3773
DOI:10.1002/anie.202401421