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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

Publication ,  Journal Article
Wells, RL; Kwag, CY; Purdy, AP; Mcphail, AT; Pitt, CG
Published in: Polyhedron
January 1, 1990

Reduction of Me3SiCH2AsCl2 (I) with LiA1H4 at -78°C afforded Me3SiCH2 AsH2 (II) and reaction of II with Ph3Ga produced [Me3SiCH2(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, [Me3SiCH2 (H)AsGaMe2]3 (IV) was produced by the reaction of II with Me3Ga; however, only H2, Me4Si, (Me3SiCH2As)5 (VI) and unreacted (Me3SiCH2)3Ga were identified after allowing the latter to react with II. Reaction of 2 equiv. of Me3SiCl with a mixture of II and n-BuLi (1 : 2 mole ratio) afforded Me3SiCH2As(SiMe3)2 (V). The monosilylated arsine was not isolated when 1 equiv. of Me3SiCl 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 (Me3SiCH2AsGaPh)n, are described. The ring compound, VI, was prepared by reaction of I with a mixture of Me3SiCl 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(C2h5)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.

Duke Scholars

Published In

Polyhedron

DOI

ISSN

0277-5387

Publication Date

January 1, 1990

Volume

9

Issue

2-3

Start / End Page

319 / 327

Related Subject Headings

  • Inorganic & Nuclear Chemistry
  • 3403 Macromolecular and materials chemistry
  • 3402 Inorganic chemistry
  • 0399 Other Chemical Sciences
  • 0306 Physical Chemistry (incl. Structural)
  • 0302 Inorganic Chemistry
 

Citation

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Wells, R. L., Kwag, C. Y., Purdy, A. P., Mcphail, A. T., & Pitt, C. G. (1990). 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. Polyhedron, 9(2–3), 319–327. https://doi.org/10.1016/S0277-5387(00)80586-0
Wells, R. L., C. Y. Kwag, A. P. Purdy, A. T. Mcphail, and C. G. Pitt. “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.” Polyhedron 9, no. 2–3 (January 1, 1990): 319–27. https://doi.org/10.1016/S0277-5387(00)80586-0.
Journal cover image

Published In

Polyhedron

DOI

ISSN

0277-5387

Publication Date

January 1, 1990

Volume

9

Issue

2-3

Start / End Page

319 / 327

Related Subject Headings

  • Inorganic & Nuclear Chemistry
  • 3403 Macromolecular and materials chemistry
  • 3402 Inorganic chemistry
  • 0399 Other Chemical Sciences
  • 0306 Physical Chemistry (incl. Structural)
  • 0302 Inorganic Chemistry