Synthesis and characterization of the neutral three-coordinate thiolate complexes Al[S(2,4,6-t-Bu3C6H2)]3 and Ga[S(2,4,6-t-Bu3C6H2)]3

Karin Ruhlandt, Philip P. Power

Research output: Contribution to journalArticle

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Abstract

The first monomeric, three-coordinate aluminum and gallium thiolate compounds have been synthesized and structurally characterized. The compounds were prepared by the reaction of the corresponding metal halide with 2 equiv of LiSMes* (Mes* = 2,4,6-t-Bu3C6H2) to give the aluminum derivative Al(SMes*)3 (1) or with 3 equiv of the lithium thiolate to give the gallium species Ga(SMes*)3 (2). The compounds were characterized by 1H NMR and infrared spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.71069 Å) radiation at 130 K: 1, Al(SMes*)3, C54H87AlS3, a = 10.229 (5) Å, b = 26.137 (7) Å, C = 19.908 (5) Å, β = 91.260 (3)°, Z = 4, monoclinic, space group F21/n, R(F) = 0.049; 2, Ga(SMes*)3, C54H87GaS3, a = 10.243 (2) Å, b = 26.189 (8) Å, c = 20.031 (3) Å, β = 91.554 (1)°, Z = 4, monoclinic, space grup P21/n, R(F) = 0.049. The structural data show that 1 and 2 have a very similar three-coordinate, almost planar, geometry at the metal. Distortions from idealized trigonal-planar coordination, as well as other structural features can be explained on the basis of ionic M-S bonding character and of some M⋯H interactions involving the o-t-Bu groups of the ligand.

Original languageEnglish (US)
Pages (from-to)2633-2637
Number of pages5
JournalInorganic Chemistry
Volume30
Issue number12
StatePublished - 1991
Externally publishedYes

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Aluminum
Gallium compounds
gallium compounds
Metal halides
aluminum
Gallium
metal halides
X ray crystallography
synthesis
Lithium
Nuclear magnetic resonance spectroscopy
crystallography
gallium
Infrared spectroscopy
lithium
Metals
infrared spectroscopy
Ligands
Derivatives
Radiation

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

Synthesis and characterization of the neutral three-coordinate thiolate complexes Al[S(2,4,6-t-Bu3C6H2)]3 and Ga[S(2,4,6-t-Bu3C6H2)]3 . / Ruhlandt, Karin; Power, Philip P.

In: Inorganic Chemistry, Vol. 30, No. 12, 1991, p. 2633-2637.

Research output: Contribution to journalArticle

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title = "Synthesis and characterization of the neutral three-coordinate thiolate complexes Al[S(2,4,6-t-Bu3C6H2)]3 and Ga[S(2,4,6-t-Bu3C6H2)]3",
abstract = "The first monomeric, three-coordinate aluminum and gallium thiolate compounds have been synthesized and structurally characterized. The compounds were prepared by the reaction of the corresponding metal halide with 2 equiv of LiSMes* (Mes* = 2,4,6-t-Bu3C6H2) to give the aluminum derivative Al(SMes*)3 (1) or with 3 equiv of the lithium thiolate to give the gallium species Ga(SMes*)3 (2). The compounds were characterized by 1H NMR and infrared spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.71069 {\AA}) radiation at 130 K: 1, Al(SMes*)3, C54H87AlS3, a = 10.229 (5) {\AA}, b = 26.137 (7) {\AA}, C = 19.908 (5) {\AA}, β = 91.260 (3)°, Z = 4, monoclinic, space group F21/n, R(F) = 0.049; 2, Ga(SMes*)3, C54H87GaS3, a = 10.243 (2) {\AA}, b = 26.189 (8) {\AA}, c = 20.031 (3) {\AA}, β = 91.554 (1)°, Z = 4, monoclinic, space grup P21/n, R(F) = 0.049. The structural data show that 1 and 2 have a very similar three-coordinate, almost planar, geometry at the metal. Distortions from idealized trigonal-planar coordination, as well as other structural features can be explained on the basis of ionic M-S bonding character and of some M⋯H interactions involving the o-t-Bu groups of the ligand.",
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N2 - The first monomeric, three-coordinate aluminum and gallium thiolate compounds have been synthesized and structurally characterized. The compounds were prepared by the reaction of the corresponding metal halide with 2 equiv of LiSMes* (Mes* = 2,4,6-t-Bu3C6H2) to give the aluminum derivative Al(SMes*)3 (1) or with 3 equiv of the lithium thiolate to give the gallium species Ga(SMes*)3 (2). The compounds were characterized by 1H NMR and infrared spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.71069 Å) radiation at 130 K: 1, Al(SMes*)3, C54H87AlS3, a = 10.229 (5) Å, b = 26.137 (7) Å, C = 19.908 (5) Å, β = 91.260 (3)°, Z = 4, monoclinic, space group F21/n, R(F) = 0.049; 2, Ga(SMes*)3, C54H87GaS3, a = 10.243 (2) Å, b = 26.189 (8) Å, c = 20.031 (3) Å, β = 91.554 (1)°, Z = 4, monoclinic, space grup P21/n, R(F) = 0.049. The structural data show that 1 and 2 have a very similar three-coordinate, almost planar, geometry at the metal. Distortions from idealized trigonal-planar coordination, as well as other structural features can be explained on the basis of ionic M-S bonding character and of some M⋯H interactions involving the o-t-Bu groups of the ligand.

AB - The first monomeric, three-coordinate aluminum and gallium thiolate compounds have been synthesized and structurally characterized. The compounds were prepared by the reaction of the corresponding metal halide with 2 equiv of LiSMes* (Mes* = 2,4,6-t-Bu3C6H2) to give the aluminum derivative Al(SMes*)3 (1) or with 3 equiv of the lithium thiolate to give the gallium species Ga(SMes*)3 (2). The compounds were characterized by 1H NMR and infrared spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.71069 Å) radiation at 130 K: 1, Al(SMes*)3, C54H87AlS3, a = 10.229 (5) Å, b = 26.137 (7) Å, C = 19.908 (5) Å, β = 91.260 (3)°, Z = 4, monoclinic, space group F21/n, R(F) = 0.049; 2, Ga(SMes*)3, C54H87GaS3, a = 10.243 (2) Å, b = 26.189 (8) Å, c = 20.031 (3) Å, β = 91.554 (1)°, Z = 4, monoclinic, space grup P21/n, R(F) = 0.049. The structural data show that 1 and 2 have a very similar three-coordinate, almost planar, geometry at the metal. Distortions from idealized trigonal-planar coordination, as well as other structural features can be explained on the basis of ionic M-S bonding character and of some M⋯H interactions involving the o-t-Bu groups of the ligand.

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