Use of organoindium hydrides for the preparation of organoindium phosphides. Synthesis and molecular structure of [(Me3CCH2)2InP(t-Bu)2]2

Abstract : The indium phosphide (Me3CCH2)2InP(t-Bu)22 has been prepared from KIn(CH2CMe3)3H and ClP(t-Bu)2 in pentane. When In(CH2CMe3)3 and HP(t-Bu)2 were present in a 1:1 mol ratio, heating to 105-115 deg C for 5 days was required, whereas when ln(CH2CMe3)3 and HP(t-Bu)2 were in a 5:1 mol ratio in pentane solution, large, colorless crystal of the desired indium product formed in 6 days at room temperature Excess phosphine, In(CH2CMe3)3 and HP(t-Bu)2 in a 1:5 mol ratio in pentane, significantly retarded the rate of formation of (Me3CCH2) 2InP(t-Bu)22. Thermal decomposition of (Me3CCH2)2InP(t-Bu)22 to form InP occurred at 245 deg C in 1 h. The compound (Me3CCH2)2InP(t-Bu)22 crystallizes in the centrosymmetric orthorhombic space group Pbcn (No. 60) with a = 11.742(3)A, b = 20.194(6)A, c = 17.909(4)A, V = 4246 (2) A3 and Z = 4. Indium-phosphorus compounds, Indium-hydrides, Single-source precursor, X-Ray structural study.