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Direct Observation by Electrospray Ionization Mass Spectrometry of
1Department of Material Science, Graduate School of Science, Osaka City University, 3-3-138 Sugimoto Sumiyoshi-ku, Osaka 558-8585 (Japan).
Angewandte Chemie (International Ed. in English)
|December 14, 1999
Summary
Methanol is crucial for synthesizing a unique double-bookshelf oxide cluster. This study identifies a key intermediate, [Cp*RhMo(3)O(8)(OMe)(5)](-), using advanced analytical techniques for its characterization.
Area of Science:
- Inorganic Chemistry
- Organometallic Chemistry
- Materials Science
Background:
- The synthesis of complex polyoxometalates often requires specific solvent conditions.
- Organometallic rhodium-molybdenum oxide clusters are of interest for their unique structures and potential applications.
Purpose of the Study:
- To investigate the formation mechanism of the double-bookshelf-type oxide cluster [(Cp*Rh)(2)Mo(6)O(20)(OMe)(2)](2-).
- To identify and characterize key intermediates in the reaction pathway.
Main Methods:
- Reaction of [{Cp*Rh(µ-Cl)Cl}(2)] with [Mo(2)O(7)](2-) in methanol.
- Electrospray ionization mass spectrometry (ESI-MS) for structural analysis.
- Deuterium labeling experiments using CD(3)OD.
Main Results:
- Methanol was identified as an essential solvent for the formation of the target cluster.
- A key intermediate, [Cp*RhMo(3)O(8)(OMe)(5)](-), was detected and its structure proposed.
- ESI-MS and labeling studies provided strong support for the proposed intermediate structure.
Conclusions:
- The reaction mechanism involves the formation of a specific rhodium-molybdenum oxide intermediate.
- Methanol plays a critical role not only as a solvent but also as a source of methoxy ligands in the cluster formation.
- The study elucidates a synthetic pathway towards complex organometallic oxide clusters.