Synthesis and characterization of pentamethylcyclopentadienylrhodium(III) and -iridium(III) complexes with 1,2-benzenedithiolate

Rimo Xi, Masaaki Abe, Takayoshi Suzuki, Takanori Nishioka, Kiyoshi Isobe

Research output: Contribution to journalArticle

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Abstract

A reaction of the triple cubane-type organometallic polyoxomolybdate cluster, [(Cp * Rh)4Mo4O16] · 2H2O (1 · 2H2O), with 1,2-benzenedithiol gives a 1,2-benzenedithiolate-bridged dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)2] (2), and another dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)(μ(S)-1,2-C6H4S(SO2)-S,S′)] (3), both of which are characterized by the single-crystal X-ray diffraction method. The former complex, 2, is also obtained from a reaction of [(Cp * RhCl)2(μ-Cl)2] with 1,2-benzenedithiol in the presence of NaOCH3, and the latter, 3, from oxygenation of 2 with t-BuOOH. The 1H NMR study in CD2Cl2 indicates that complex 2 changes gradually to a coordinatively unsaturated mononuclear complex, [Cp * Rh(1,2-C6H4S2-S,S′)] (4). An analogous mononuclear iridium(III) complex, [Cp * Ir(1,2-C6H4S2-S,S′)] (5), is also prepared and characterized by X-ray structural analysis.

Original languageEnglish
Pages (from-to)117-125
Number of pages9
JournalJournal of Organometallic Chemistry
Volume549
Issue number1-2
Publication statusPublished - Dec 18 1997
Externally publishedYes

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Iridium
Oxygenation
Organometallics
iridium
Structural analysis
Nuclear magnetic resonance
Single crystals
cubane
X ray diffraction
X rays
oxygenation
synthesis
structural analysis
X-Ray Diffraction
x rays
X-Rays
nuclear magnetic resonance
single crystals
diffraction
1,2-benzenedithiol

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Organic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

Synthesis and characterization of pentamethylcyclopentadienylrhodium(III) and -iridium(III) complexes with 1,2-benzenedithiolate. / Xi, Rimo; Abe, Masaaki; Suzuki, Takayoshi; Nishioka, Takanori; Isobe, Kiyoshi.

In: Journal of Organometallic Chemistry, Vol. 549, No. 1-2, 18.12.1997, p. 117-125.

Research output: Contribution to journalArticle

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abstract = "A reaction of the triple cubane-type organometallic polyoxomolybdate cluster, [(Cp * Rh)4Mo4O16] · 2H2O (1 · 2H2O), with 1,2-benzenedithiol gives a 1,2-benzenedithiolate-bridged dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)2] (2), and another dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)(μ(S)-1,2-C6H4S(SO2)-S,S′)] (3), both of which are characterized by the single-crystal X-ray diffraction method. The former complex, 2, is also obtained from a reaction of [(Cp * RhCl)2(μ-Cl)2] with 1,2-benzenedithiol in the presence of NaOCH3, and the latter, 3, from oxygenation of 2 with t-BuOOH. The 1H NMR study in CD2Cl2 indicates that complex 2 changes gradually to a coordinatively unsaturated mononuclear complex, [Cp * Rh(1,2-C6H4S2-S,S′)] (4). An analogous mononuclear iridium(III) complex, [Cp * Ir(1,2-C6H4S2-S,S′)] (5), is also prepared and characterized by X-ray structural analysis.",
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N2 - A reaction of the triple cubane-type organometallic polyoxomolybdate cluster, [(Cp * Rh)4Mo4O16] · 2H2O (1 · 2H2O), with 1,2-benzenedithiol gives a 1,2-benzenedithiolate-bridged dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)2] (2), and another dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)(μ(S)-1,2-C6H4S(SO2)-S,S′)] (3), both of which are characterized by the single-crystal X-ray diffraction method. The former complex, 2, is also obtained from a reaction of [(Cp * RhCl)2(μ-Cl)2] with 1,2-benzenedithiol in the presence of NaOCH3, and the latter, 3, from oxygenation of 2 with t-BuOOH. The 1H NMR study in CD2Cl2 indicates that complex 2 changes gradually to a coordinatively unsaturated mononuclear complex, [Cp * Rh(1,2-C6H4S2-S,S′)] (4). An analogous mononuclear iridium(III) complex, [Cp * Ir(1,2-C6H4S2-S,S′)] (5), is also prepared and characterized by X-ray structural analysis.

AB - A reaction of the triple cubane-type organometallic polyoxomolybdate cluster, [(Cp * Rh)4Mo4O16] · 2H2O (1 · 2H2O), with 1,2-benzenedithiol gives a 1,2-benzenedithiolate-bridged dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)2] (2), and another dinuclear complex, [(Cp * Rh)2(μ(S)-1,2-C6H4S2-S,S′)(μ(S)-1,2-C6H4S(SO2)-S,S′)] (3), both of which are characterized by the single-crystal X-ray diffraction method. The former complex, 2, is also obtained from a reaction of [(Cp * RhCl)2(μ-Cl)2] with 1,2-benzenedithiol in the presence of NaOCH3, and the latter, 3, from oxygenation of 2 with t-BuOOH. The 1H NMR study in CD2Cl2 indicates that complex 2 changes gradually to a coordinatively unsaturated mononuclear complex, [Cp * Rh(1,2-C6H4S2-S,S′)] (4). An analogous mononuclear iridium(III) complex, [Cp * Ir(1,2-C6H4S2-S,S′)] (5), is also prepared and characterized by X-ray structural analysis.

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