Synthesis and Characterization of Oxygen/Sulfur-Bridged Incomplete Cubane-Type Clusters, [M₃S₄(Tpe)₃]⁺ and [M₃OS₃(Tpe)₃]⁺ (M = Mo and W), and a Mixed-Metal Cubane-Type Cluster, [Mo₃PdS₄Cl(Tpe)₃]
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- Yoshida Ryouichi
- Research Institute for Natural Sciences, Okayama University of Science
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- Shibahara Takashi
- Department of Chemistry, Okayama University of Science
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- Akashi Haruo
- Research Institute for Natural Sciences, Okayama University of Science
書誌事項
- タイトル別名
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- Synthesis and Characterization of Oxygen/Sulfur-Bridged Incomplete Cubane-Type Clusters, [M<sub>3</sub>S<sub>4</sub>(Tpe)<sub>3</sub>]<sup>+</sup> and [M<sub>3</sub>OS<sub>3</sub>(Tpe)<sub>3</sub>]<sup>+</sup> (M = Mo and W), and a Mixed-Metal Cubane-Type Cluster, [Mo<sub>3</sub>PdS<sub>4</sub>Cl(Tpe)<sub>3</sub>]
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The reaction of [Mo3S4(H2O)9]4+ (1) and [Mo3OS3(H2O)9]4+ (2) with hydrotris(pyrazolyl)ethanol (HTpe) ligands produced [Mo3S4(Tpe)3]PF6·3CH2Cl2 ([5]PF6·3CH2Cl2) and [Mo3OS3(Tpe)3]PF6·4CH2Cl2 ([6]PF6·4CH2Cl2), respectively, using solvent extraction. Furthermore, the tungsten analogous compounds, [W3S4(Tpe)3]PF6·4CH2Cl2 ([7]PF6·4CH2Cl2) and [W3OS3(Tpe)3]PF6·2.5CH2Cl2 ([8]PF6·2.5CH2Cl2) have been prepared using a similar procedure to that used in the preparation of 5. The cyclic voltammograms of 5, 6, and 7 show one reversible one-electron oxidation process and one reversible one-electron reduction process (5, E1/2 = −0.96 and 1.10 V; 6, E1/2 = −0.96 and 1.00 V; 7, E1/2 = −1.54 and 0.77 V: all values are given vs. SHE). Complex 8 also shows one reversible (E1/2 = 0.61 V) and one irreversible one-electron oxidation processes (Epc = 1.12 V) and one irreversible one-electron reduction process (Epc = −1.54 V). The reaction of 5 with organometallic compound [Pd2(dba)3] in CH3CN afforded [Mo3PdS4Cl(Tpe)3]·4.5CH2Cl2 ([11]·4.5CH2Cl2). Complex 11 showed a high catalytic activity for the intramolecular cyclization of 4-pentynoic acid to give γ-methylene-γ-butyrolactone in the presence of Et3N. X-ray structure analyses of [5]PF6·3CH2Cl2, [6]PF6·4CH2Cl2, [7]PF6·4CH2Cl2, [8]PF6·2.5CH2Cl2, and [11]·4.5CH2Cl2 revealed that each molybdenum or tungsten atom is bonded to the Tpe ligand.
収録刊行物
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- Bulletin of the Chemical Society of Japan
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Bulletin of the Chemical Society of Japan 86 (7), 839-849, 2013
公益社団法人 日本化学会
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詳細情報 詳細情報について
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- CRID
- 1390001204143526656
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- NII論文ID
- 10031183248
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- NII書誌ID
- AA00580132
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- COI
- 1:CAS:528:DC%2BC3sXht1ClsbrJ
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- ISSN
- 13480634
- 00092673
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- NDL書誌ID
- 024672028
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- 本文言語コード
- en
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- データソース種別
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- JaLC
- NDL
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