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High‐Pressure Synthesis, Crystal Structure, and Characterization of Zn 2 PN 3 – A New catena ‐Polynitridophosphate
Author(s) -
Sedlmaier Stefan J.,
Eberspächer Moritz,
Schnick Wolfgang
Publication year - 2011
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201000403
Subject(s) - raman spectroscopy , microcrystalline , crystal structure , crystallography , rietveld refinement , chemistry , zinc , powder diffraction , ion , infrared spectroscopy , physics , organic chemistry , optics
Phase‐pure zinc catena ‐polynitridophosphate Zn 2 PN 3 was synthesized by means of high‐pressure high‐temperature conditions (1200 °C, 8 GPa) starting from Zn 3 N 2 and P 3 N 5 utilizing a multianvil assembly. It was obtained as a colorless, microcrystalline powder. The crystal structure of Zn 2 PN 3 ( Cmc 2 1 , no. 36, a = 937.847(6), b = 547.696(4), c = 492.396(3) pm, Z = 4, R p = 0.0110, wR p = 0.0141) has been refined from powder X‐ray diffraction data by the Rietveld method using the atomic parameters of isotypic Mg 2 PN 3 as starting values. Interconnected by N‐coordinated Zn 2+ ions, the catena ‐polynitridophosphate chain anions run parallel [001] with a chain periodicity P = 2 and a stretching factor f s = 0.88. FT‐IR and Raman spectra of Zn 2 PN 3 were recorded and relevant bands were assigned. The solid‐state 31 P MAS NMR spectrum yielded a single resonance at δ = 42.8. In addition an account of the thermal behavior of Zn 2 PN 3 is given.