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The Stuffed Framework Structure of SrP 2 N 4 : Challenges to Synthesis and Crystal Structure Determination
Author(s) -
Karau Friedrich W.,
Seyfarth Lena,
Oeckler Oliver,
Senker Jürgen,
Landskron Kai,
Schnick Wolfgang
Publication year - 2007
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.200700216
Subject(s) - crystallography , crystal structure , powder diffraction , synchrotron , neutron diffraction , rietveld refinement , diffraction , materials science , chemistry , physics , optics
SrP 2 N 4 was obtained by high‐pressure high‐temperature synthesis utilizing the multianvil technique (5 GPa, 1400 °C) starting from mixtures of phosphorus(V) nitride and strontium azide. SrP 2 N 4 turned out to be isotypic with BaGa 2 O 4 and is closely related to KGeAlO 4 . The crystal structure (SrP 2 N 4 , a =17.1029(8), c =8.10318(5) Å, space group P 6 3 (no. 173), V =2052.70(2) Å 3 , Z =24, R ( F 2 )=0.0633) was solved from synchrotron powder diffraction data by applying a combination of direct methods, Patterson syntheses, and difference Fourier maps adding the unit cell information derived from electron diffraction and symmetry information obtained from 31 P solid‐state NMR spectroscopy. The structure of SrP 2 N 4 was refined by the Rietveld method by utilizing both neutron and synchrotron X‐ray powder diffraction data, and has been corroborated additionally by 31 P solid‐state NMR spectroscopy by employing through‐bond connectivities and distance relations.