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Issue 6, 2002
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Rhodium(III) complexes with thiolate and thioether ligands derived from fac(S)-[Rh(aet)3] (aet = 2-aminoethanethiolate): selective formation, characterization and properties

Masakazu Hirotsu,a  Atsushi Kobayashi,a  Takashi Yoshimuraa  and  Takumi Konno*b 
Author affiliations

* Corresponding authors

a Department of Chemistry, Faculty of Engineering, Gunma University, Kiryu, Japan

b Department of Chemistry, Graduate School of Science, Osaka University, Toyonaka, Japan
E-mail: konno@ch.wani.osaka-u.ac.jp

Abstract

Alkylation of fac(S)-[Rh(aet)3] (aet = NH2CH2CH2S−) with use of 1,2-dibromoethane in N,N-dimethylformamide produces fac(S)-[Rh(aet)(baete)]2+ ([1]2+, baete = (NH2CH2CH2SCH2)2), in which two of the three thiolato S atoms in fac(S)-[Rh(aet)3] are linked by an ethylene group. When methyl iodide is used as an alkylating reagent, two of the three thiolato S atoms are methylated to give fac(S)-[Rh(aet)(mtea)2]2+ ([2]2+, mtea = NH2CH2CH2SCH3). Complexes [1]2+ and [2]2+ were optically resolved into the two enantiomers by SP-Sephadex C-25 column chromatography. The synthesis of a trimethylated complex, fac(S)-[Rh(mtea)3]3+ ([3]3+), has been achieved by treatment of an aqueous solution of [2]2+ with dimethyl sulfate. Reactions of [1]2+ or [2]2+ with Ag+ in a 2 ∶ 1 molar ratio in water produce S-bridged RhIIIAgIRhIII trinuclear complexes, [Ag{Rh(aet)(baete)}2]5+ ([4]5+) and [Ag{Rh(aet)(mtea)2}2]5+ ([5]5+), indicating that [1]2+ and [2]2+ act as an S-donating monodentate complex-ligand. These complexes have been characterized by UV-VIS absorption, CD and NMR spectroscopic methods, together with single-crystal X-ray analyses for [1]2+ and [3]3+.

Graphical abstract: Rhodium(iii) complexes with thiolate and thioether ligands derived from fac(S)-[Rh(aet)3] (aet = 2-aminoethanethiolate): selective formation, characterization and properties

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Publication details

The article was received on 03 Sep 2001, accepted on 30 Nov 2001 and first published on 11 Feb 2002


Article type: Paper
DOI: 10.1039/B107933F
Citation: J. Chem. Soc., Dalton Trans., 2002,0, 878-884
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    Rhodium(III) complexes with thiolate and thioether ligands derived from fac(S)-[Rh(aet)3] (aet = 2-aminoethanethiolate): selective formation, characterization and properties

    M. Hirotsu, A. Kobayashi, T. Yoshimura and T. Konno, J. Chem. Soc., Dalton Trans., 2002, 0, 878
    DOI: 10.1039/B107933F

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