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Publication Detail
Synthetic and Structural Studies of Donor-Functionalized Alkoxy Derivatives of Gallium
  • Publication Type:
    Journal article
  • Publication Sub Type:
    Article
  • Authors:
    Knapp CE, Pugh D, McMillan PF, Parkin IP, Carmalt CJ
  • Publisher:
    AMER CHEMICAL SOC
  • Publication date:
    03/10/2011
  • Pagination:
    9491, 9498
  • Journal:
    INORG CHEM
  • Volume:
    50
  • Issue:
    19
  • Print ISSN:
    0020-1669
  • Language:
    EN
  • Keywords:
    CHEMICAL-VAPOR-DEPOSITION, OXIDE THIN-FILMS, CATALYZED CROSS-METHYLATION, ALKYL METAL ALKOXIDES, VIBRATIONAL-SPECTRA, GAS SENSORS, ALUMINUM, INDIUM, PRECURSORS, COMPLEXES
  • Addresses:
    Carmalt, CJ
    UCL
    Dept Chem
    Mat Chem Ctr
    London
    WC1H 0AJ
    England
Abstract
The synthesis of a range of alkyl/chloro-gallium alkoxide and amido/alkoxide compounds was achieved via a series of protonolysis and alcoholysis steps. The initial reaction involved the synthesis of [Me(Cl)Ga{N(SiMe3)(2)}](2) (1) via methyl group transfer from the reaction of GaCl3 with two equivalents of LiN(SiMe3)(2). Reaction of 1 with varying amounts of ROH resulted in the formation of [Me(Cl)Ga(OR)](2) (2, R = CH2CH2OMe; 3, CH(CH3)CH2NMe2), [Me(Cl)Ga{N(SiMe3)(2)} (mu(2)-OR)Ga(Cl)Me] (4, R = CH2CH2NMe2), or [MeGa(OR)(2)] (5, R = CH(CH3)CH2NMe2). Compound 4 represents an intermediate in the formation of dimeric complexes, of the type [Me(Cl)Ga(OR)](2), when formed from compound [Me(Cl)Ga{N(SiMe3)(2)}](2). A methylgallium amido/alkoxide complex [MeGa{N(SiMe3)(2)} (OCH2CH2OMe)](2) (6) was isolated when 2 was further reacted with LiN(SiMe3)(2). In addition, reaction of 2 with (HOBu)-Bu-t resulted in a simple alcohol/alkoxide exchange and formation of [Me(Cl)Ga((OBu)-Bu-t)](2) (7). In contrast to the formation of 1, the in situ reaction of GaCl3 with one equivalent of LiN(SiMe3)(2) yielded [Cl2Ga{N(SiMe3)(2)}](2) in low yield, where no methyl group transfer has occurred. Reaction of alcohol with [Cl2Ga{N(SiMe3)(2)}](2) was then found to yield [Cl2Ga(OR)](2) (8, R = CH2CH2NMe2), and further reaction of 8 with LiN(SiMe3)(2) yielded the gallium amido alkcodde complex, [ClGa{N(SiMe3)(2)}(OR)](2) (9, R = CH2CH2NMe2), similar to 6. The structures of compounds 4, 5, 7, and 8 have been determined by single-crystal X-ray diffraction.
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