Synthesis and Characterization of Gallium and Indium Thiolate Complexes. Crystal and Molecular Structures of [M(SC5H4N)3] (M = Ga, In), [In(SC5H3N-3-SiMe3)3], and [M2(OC2H4)2(SC5H4N)4] (M = Ga, In)

David J. Rose, Yuan Da Chang, Qin Chen, Peter B. Kettler, Jon Zubieta

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58 Scopus citations

Abstract

The synthesis and characterizations of the monomeric group III thiolate complexes [In(SC5H4N)3] (1), [In(SC5H3N-3-SiMe3)3] (2), and [Ga(SC5H4N)3] (5) and of the binuclear alkoxy-bridged derivatives [M2(OC2H5)2(SC5H4N)4] (M = In (3), Ga (6)) are described. Compounds 1 and 2 are formed in the reaction of the appropriate nitrate salt M(NO3)3xH2O with the pyridine-2-thiol derivative in ethanol or water in the presence of triethylamine. In contrast, when the reaction is carried out under strictly anaerobic conditions, using the appropriate metal chloride MCl3 in ethanol solution, the binuclear species 3 and 6 are obtained. Compound 5 was prepared using GaCl3 in THF with pyridine-2-thiol under strictly anaerobic conditions. Compound 4 was prepared under anaerobic conditions in THF solvent from GaCl3 and pyridine-2-thiol. Attempts to prepare complexes of the 3,6-bis(tert-butyldimethylsilyl)pyridine-2-thiol ligand type were unsuccessful. However, the sodium salt [Na{SC5H2N-3,6-(SiMe2But)2}]6•2(C2H5)2O (7) was isolated and the structure characterized. Crystal data: 1, C15H12N3S3In, monoclinic, P21 a = 8.779(2) Å, b = 11.614(2) Å, c = 9.397(2) Å, ß = 114.67(3)°, V = 870.7(4) Å3, Z = 2, 2392 reflections with Io > 3σ (Io), R = 0.0338; 2, C24H36N3S3Si3In, orthorhombic, Pca21, a = 11.645(2) Å, b = 19.741(4) Å, c = 14.040(3) Å, V = 3227(2) Å3, Z = 4, 1930 reflections, R = 0.0464; 3, C24H26N4O2S4ln2, monoclinic, P2/n, a = 8.420(2) Å, b= 11.860(2) Å, c = 14.629(3) Å, ß = 101.83(3)°, V = 1429.8(7) Å3, Z = 2, 1699 reflections, R = 0.0296; 5, C15H12N3S3Ga, monoclinic, P21/n, a = 8.661(2) Å, b = 11.609(4) Å, c = 9.315(2) Å, ß= 115.40(3) Å, Z = 2, 1508 reflections, R = 0.0453; 6, C24H26N4O2S4Ga2, monoclinic, P21/n, a = 8.444(2) Å, b = 11.497(2) Å, c = 14.162(3) Å, ß = 1354.4(7)°, Z = 2, 1513 reflections, R = 0.0349; 7, C124H248N6OS6Si12Na6, triclinic, P1, a = 16.156(3) Å, c = 17.665(4) Å, α = 118.47(3)°, ß = 92.40(3)°, γ = 114.75(3)°, V = 3757(2) Å3, Z = 1, 5125 reflections, R = 0.0809.

Original languageEnglish (US)
Pages (from-to)3973-3979
Number of pages7
JournalInorganic Chemistry
Volume34
Issue number15
DOIs
StatePublished - Jul 1 1995

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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