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M H 4 P 6 N 12 ( M =Mg, Ca): New Imidonitridophosphates with an Unprecedented Layered Network Structure Type
Author(s) -
Marchuk Alexey,
Celinski Vinicius R.,
Schmedt auf der Günne Jörn,
Schnick Wolfgang
Publication year - 2015
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.201406240
Subject(s) - crystallography , crystal structure , stoichiometry , amorphous solid , alkali metal , single crystal , materials science , alkaline earth metal , rietveld refinement , metal , spectroscopy , chemistry , physics , organic chemistry , quantum mechanics , metallurgy
Isotypic imidonitridophosphates M H 4 P 6 N 12 ( M =Mg, Ca) have been synthesized by high‐pressure/high‐temperature reactions at 8 GPa and 1000 °C starting from stoichiometric amounts of the respective alkaline‐earth metal nitrides, P 3 N 5 , and amorphous HPN 2 . Both compounds form colorless transparent platelet crystals. The crystal structures have been solved and refined from single‐crystal X‐ray diffraction data. Rietveld refinement confirmed the accuracy of the structure determination. In order to quantify the amounts of H atoms in the respective compounds, quantitative solid‐state 1 H NMR measurements were carried out. EDX spectroscopy confirmed the chemical compositions. FTIR spectra confirmed the presence of NH groups in both structures. The crystal structures reveal an unprecedented layered tetrahedral arrangement, built up from all‐side vertex‐sharing PN 4 tetrahedra with condensed dreier and sechser rings. The resulting layers are separated by metal atoms.