Publications [#233197] of Andrew T. McPhail
Journal Articles
- Wells, RL; Kwag, CY; Purdy, AP; Mcphail, AT; Pitt, CG, "Preparation and chemistry of Me3SiCH2AsH2; Preparation of [Me3SiCH2(H)AsGaPh2]3, a trimeric mono(arsino)gallane containing a hydrogen bonded to arsenic. Isolation and X-ray crystal structure of (Me3SiCH2As)5", PolyhedronJanuary,, 1990, 9(2-3), 319-327, Elsevier BV [Gateway.cgi], [doi].
(last updated on 2026/01/21)Abstract:
Reduction of Me3 SiCH2 AsCl2 (I) with LiA1H4 at -78°C afforded Me3 SiCH2 AsH2 (II) and reaction of II with Ph3 Ga produced [Me3 SiCH2 (H)AsGaPh2 ]3 (III) which was characterized by partial elemental analysis (C and H), 1H NMR spectroscopy and a cryoscopic molecular weight determination. Based on 1H NMR data, [Me3 SiCH2 (H)AsGaMe2 ]3 (IV) was produced by the reaction of II with Me3 Ga; however, only H2 , Me4 Si, (Me3 SiCH2 As)5 (VI) and unreacted (Me3 SiCH2 )3 Ga were identified after allowing the latter to react with II. Reaction of 2 equiv. of Me3 SiCl with a mixture of II and n-BuLi (1 : 2 mole ratio) afforded Me3 SiCH2 As(SiMe3 )2 (V). The monosilylated arsine was not isolated when 1 equiv. of Me3 SiCl was allowed to react with combined II and n-BuLi (1 : 1 mole ratio); rather, a mixture of II and V resulted. Attempted preparations of (Me3 SiCH2 AsGaPh)n , are described. The ring compound, VI, was prepared by reaction of I with a mixture of Me3 SiCl and Mg in THF. The molecular structure of this cycloarsane was determined by single-crystal X-ray diffraction methods. Pale yellow crystals of VI belong to the monoclinic system with four molecules occupying the general positions of space group P21 /c(C2h 5)with cell constants: a = 9.952(1), b = 30.245(9), c = 13.000(3) Å, β = 91.69(1)°, V = 3911.3 Å 3, Z = 4. © 1990.