Abstract
AbstractThe Reduced Nitridosilicate BaSi6N8The reduced nitridosilicate BaSi6N8 has been synthesized starting from barium nitride and silicon diimide in a radio‐frequency furnace at temperatures of about 1650 °C. The structure has been determined from X‐ray powder diffraction data and was refined by the Rietveld method (Imm2 (no. 44), a = 793.16(1), b = 934.37(2), c = 483.57(1) pm, V = 358.38(1) ·106 pm3, Z = 2, wRp = 0.0353, Rp = 0.0238, RF2 = 0.0660, 452 observed reflections, 42 parameters). BaSi6N8 crystallizes isotypically with SrSi6N8. The three‐dimensional Si‐N‐network consists of corner‐sharing SiN4 tetrahedra and single bonds Si‐Si forming N3Si‐SiN3 building units. 29Si solid‐state NMR spectra of BaSi6N8 resemble those of SrSi6N8 exhibiting two resonances at δ = −54.3 and −28.0 ppm. Their observed intensity ratio of approximately 2 : 1 can be attributed to the SiN4 tetrahedra and the Si2N6 units, respectively. This observation is in accordance with the results from the X‐ray structure determination (Si at Wyckoff positions 8e (SiN4) and 4d (Si2N6)).
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