Synthese und Kristallstruktur des Kalium‐Iminophosphanids [K4(THF)3(Me3SiNPEt2)2(OSiMe2OSiMe2O)]2

Abstract

The potassium iminophosphanide complex [K4(thf)3(Me3SiNPEt2)2(OSiMe2OSiMe2O)]2 has been obtained by a melt reaction of Me3SiNPEt3 with potassium hydride at 140 °C in the presence of silicon grease (—OSiMe2—)n and subsequent crystallization from thf solution. The colourless moisture sensitive single crystals are characterized by X‐ray diffraction: Space group P1¯, Z = 1, lattice dimensions at —70 °C: a = 1135.9(3), b = 1250.0(3), c = 1866.1(4) pm, α = 92.65(1)°, β = 100.80(1)°, γ = 93.57(1)°, R1 = 0.0604. The centrosymmetric dimeric cluster aggregate is formed by two of the eight potassium ions which are connected with the central oxygen atom of both the (OSiMe2OSiMe2O)2— chains as well as with one of their terminal O atoms each. The remaining potassium ions are connected with the phosphorus atoms of the iminophosphanide groups (Me3SiNPEt2)— as well as with its nitrogen atoms. They are terminally solvated by thf molecules.