The Long-Periodic Loop-Branched Chain Structure of the Oxonitridophosphate La 21 P 40 O 46 N 57 , Elucidated by a Combination of TEM and Microfocused Synchrotron Radiation

The lanthanum oxonitridophosphate La P O N was synthesized by high-pressure metathesis from partially hydrolysed LiPN and LaCl at 750-950 °C and 7-9 GPa. The combination of transmission electron microscopy (TEM) and diffraction using microfocused synchrotron radiation revealed a monoclinic crystal s...

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Veröffentlicht in:Chemistry : a European journal 2019-11, Vol.25 (63), p.14382-14387
Hauptverfasser: Nentwig, Markus, Kloß, Simon D, Neudert, Lukas, Eisenburger, Lucien, Schnick, Wolfgang, Oeckler, Oliver
Format: Artikel
Sprache:eng
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Zusammenfassung:The lanthanum oxonitridophosphate La P O N was synthesized by high-pressure metathesis from partially hydrolysed LiPN and LaCl at 750-950 °C and 7-9 GPa. The combination of transmission electron microscopy (TEM) and diffraction using microfocused synchrotron radiation revealed a monoclinic crystal structure (space group P2 /n, a=14.042(4), b=7.084(3), c=41.404(10) Å, β=97.73(3)° and Z=2), which is characterized by loop-branched 21 member single chains of P(O,N) tetrahedra that extend along [2 0 1]. These chains are related to the loop-branched dreier single chains with dreier-ring loops in stillwellite (CeBSiO ). In La P O N , these chains are characterized by a complex long-periodic conformation and exhibit disorder that involves La/N and P split positions. This is an extraordinarily long periodicity with respect to branched single chains of tetrahedra. La P O N constitutes the first rare-earth oxonitridophosphate exhibiting a chain structure. Single-crystal data are consistent with electron and powder X-ray diffraction.
ISSN:0947-6539
1521-3765
DOI:10.1002/chem.201902873