Synthesis, Structure and CVD Studies of the Group 13 Complexes [Me2M{tfacnac}] [M = Al, Ga, In; Htfacnac = F3CC(OH)CHC(CH3)NCH2CH2OCH3]

Samuel D. Cosham, Jeff A. Hamilton, Michael S. Hill, Andrew L. Johnson, Kieran C. Molloy

Research output: Contribution to journalArticle

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Abstract

A family of group 13 metal dimethyl complexes of the general form [Me2M{ MeC(O)CHC(NCH2CH2OMe)CF3}] (M = Al (2), Ga (3) or In (4)) have been synthesised by reaction of the isolated free ligand (1) with the corresponding trimethyl-metal reagents. The isolated complexes (2-4) were characterised by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction which reveals the compounds to be monomeric 5 coordinate complexes with coordination of the pendent ether bearing lariat in the solid state. Thermogravimetric analysis showed complexes 2-4 all to have residual masses, at 200 °C, of 2.4% or less well below the value for the respective metal oxides, and vapour pressure measurements show the indium complex (4) to be an order of magnitude less volatile (0.09 Torr at 80 oC) than the Al (2) or Ga (3) derivatives despite being isoleptic systems. Complexes 2-4 have all been investigated for their utility in the LP-MOCVD growth of the respective metal oxides in the absence of additional oxidant at 400 °C on silicon substrates.
LanguageEnglish
Pages1712-1719
JournalEuropean Journal of Inorganic Chemistry
Volume2016
Issue number11
Early online date18 Mar 2016
DOIs
StatusPublished - Apr 2016

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Chemical vapor deposition
Metals
Oxides
Bearings (structural)
Indium
Metallorganic chemical vapor deposition
Silicon
Pressure measurement
Vapor pressure
Oxidants
Ether
Molecular structure
Nuclear magnetic resonance spectroscopy
Thermogravimetric analysis
Single crystals
Ligands
Derivatives
X ray diffraction
Substrates
Chemical analysis

Keywords

  • Aluminium
  • Gallium
  • Indium
  • Oxides, Chemical Vapour Deposition.

Cite this

Synthesis, Structure and CVD Studies of the Group 13 Complexes [Me2M{tfacnac}] [M = Al, Ga, In; Htfacnac = F3CC(OH)CHC(CH3)NCH2CH2OCH3]. / Cosham, Samuel D.; Hamilton, Jeff A.; Hill, Michael S.; Johnson, Andrew L.; Molloy, Kieran C.

In: European Journal of Inorganic Chemistry, Vol. 2016, No. 11, 04.2016, p. 1712-1719.

Research output: Contribution to journalArticle

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abstract = "A family of group 13 metal dimethyl complexes of the general form [Me2M{ MeC(O)CHC(NCH2CH2OMe)CF3}] (M = Al (2), Ga (3) or In (4)) have been synthesised by reaction of the isolated free ligand (1) with the corresponding trimethyl-metal reagents. The isolated complexes (2-4) were characterised by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction which reveals the compounds to be monomeric 5 coordinate complexes with coordination of the pendent ether bearing lariat in the solid state. Thermogravimetric analysis showed complexes 2-4 all to have residual masses, at 200 °C, of 2.4{\%} or less well below the value for the respective metal oxides, and vapour pressure measurements show the indium complex (4) to be an order of magnitude less volatile (0.09 Torr at 80 oC) than the Al (2) or Ga (3) derivatives despite being isoleptic systems. Complexes 2-4 have all been investigated for their utility in the LP-MOCVD growth of the respective metal oxides in the absence of additional oxidant at 400 °C on silicon substrates.",
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N2 - A family of group 13 metal dimethyl complexes of the general form [Me2M{ MeC(O)CHC(NCH2CH2OMe)CF3}] (M = Al (2), Ga (3) or In (4)) have been synthesised by reaction of the isolated free ligand (1) with the corresponding trimethyl-metal reagents. The isolated complexes (2-4) were characterised by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction which reveals the compounds to be monomeric 5 coordinate complexes with coordination of the pendent ether bearing lariat in the solid state. Thermogravimetric analysis showed complexes 2-4 all to have residual masses, at 200 °C, of 2.4% or less well below the value for the respective metal oxides, and vapour pressure measurements show the indium complex (4) to be an order of magnitude less volatile (0.09 Torr at 80 oC) than the Al (2) or Ga (3) derivatives despite being isoleptic systems. Complexes 2-4 have all been investigated for their utility in the LP-MOCVD growth of the respective metal oxides in the absence of additional oxidant at 400 °C on silicon substrates.

AB - A family of group 13 metal dimethyl complexes of the general form [Me2M{ MeC(O)CHC(NCH2CH2OMe)CF3}] (M = Al (2), Ga (3) or In (4)) have been synthesised by reaction of the isolated free ligand (1) with the corresponding trimethyl-metal reagents. The isolated complexes (2-4) were characterised by elemental analysis, NMR spectroscopy, and the molecular structures of the complexes were determined by single crystal X-ray diffraction which reveals the compounds to be monomeric 5 coordinate complexes with coordination of the pendent ether bearing lariat in the solid state. Thermogravimetric analysis showed complexes 2-4 all to have residual masses, at 200 °C, of 2.4% or less well below the value for the respective metal oxides, and vapour pressure measurements show the indium complex (4) to be an order of magnitude less volatile (0.09 Torr at 80 oC) than the Al (2) or Ga (3) derivatives despite being isoleptic systems. Complexes 2-4 have all been investigated for their utility in the LP-MOCVD growth of the respective metal oxides in the absence of additional oxidant at 400 °C on silicon substrates.

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