Bei der Reaktion von SnI4 mit KNH2 in flüssigem Ammoniak bei 243 K entsteht ein weißes Produktgemenge. Nach Abdampfen des Ammoniaks wurde der feste Rückstand 2–5 d bei 573 K im Vakuum getempert. Anschließend aufgenommene Röntgen‐Pulverdiffraktogramme zeigten Reflexe von KI und einer neuen Verbindung Sn3N4. Analoge Reaktionen von SnBr2 mit KNH2 führten neben KBr ebenfalls zu schwarzbraunem, mikrokristallinem Sn3N4 und zusätzlich zu metallischem Zinn.
Die Struktur von Zinn(IV)‐nitrid wurde anhand von Röntgen‐ und Neutronenpulverdiffraktometrie geklärt: Raumgruppe Fd 3 m, Z = 8, a = 9,037(3) Å.
Sn3N4 kristallisiert in einer Spinell‐Struktur. Beide Metallatom‐Positionen sind von Zinnatomen in der Oxidationsstufe +4 besetzt.
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Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl‐Anions: The Compound [Li(NH3)4]2[Sn2Ph4]
Ruby‐red, brittle single crystals of [Li(NH3)4]2[Sn2Ph4] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at −35°C. The structure was determined from X‐ray singlecrystal diffractometer data: Space group, P1, Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R1 (F 02 ⩾ 4σF 02) = 5.13%, wR2 (F02 ⩾ 4σF 02) = 10.5%, N(F 02 ⩾ 4σF 02) = 779, N(Var.) = 163.
The compound contains to Sb2Ph4 isosteric centres [Sn2Ph4]2− as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c‐plane, but stacked along [100].
Tin nitrides (Sn3N4) prepared by the reaction of Sn-halides with KNH2 in liquid ammonia and a subsequent vacuum annealing procedure were investigated with transmission mode XAFS experiments. While the near edge data suggest the presence of a univalent Sn-compound with a valency close to +4, the analysis of the extended X-ray absorption fine structure proves the presence of two different local Sn sites in this crystal structure: While Sn(1) is surrounded by 4 nitrogen in a distance of 2.06 A, each Sn(2) ion is coordinated with 6 nitrogen at about 2.17 A radial distance.
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