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- Title
An Update on W<sup>II</sup> and Mo<sup>II</sup> Carbonyl Precursors and Their Application in the Synthesis of Potentially Bio-Inspired Thiophenolate-Oxazoline Complexes.
- Authors
Peschel, Lydia M.; Schachner, Jörg A.; Sala, Chris H.; Belaj, Ferdinand; Mösch‐Zanetti, Nadia C.
- Abstract
The synthesis of two new low-valent dicarbonyl complexes of tungsten [W(CO)2(SPh-oz)2] ( 3b) and molybdenum [Mo(CO)2(SPh-oz)2] ( 4b) coordinated by a bidentate thiolate-oxazoline ligand SPh-oz is reported. The thereby created coordination via two anionic sulfur atoms can be seen as biologically inspired as it reflects the first coordination sphere of the pterin cofactor found in molybdenum and tungsten enzymes. The in-situ preparation of the lithium salt Li(SPh-oz) (1) was described previously in literature, but analytical data was not available. A similar situation was found for the published syntheses of the low-valent metal precursors [W(CO)3(PPh3)2Cl2] (2a), [W2(CO)7Br4] (3a) and [Mo(CO)4Br2] where experimental procedures were unreliable and experimental data was inadequate or missing.To the best of our knowledge this is the first report of a full characterization of the literature known compounds Li(SPh-oz) (1), [W(CO)3(PPh3)2Cl2] ( 2a) and [W2(CO)7Br4] ( 3a). Furthermore the novel tetranuclear Mo-precursor [Mo4(CO)7Br10] ( 4a) was synthesized. The symmetric and asymmetric IR stretching frequencies of its seven carbonyl ligands were calculated using DFT and related to the experimental values. The molecular structures of the novel precursor compounds [W(CO)2(PPh3)2Cl2] ( 2a'), [PPh3Cl]2[WCl6] ( 2b), [Mo4(CO)7Br10] ( 4a), the two complexes with the SPh-oz ligand [W(CO)2(SPh-oz)2] ( 3b), [Mo(CO)2(SPh-oz)2] ( 4b) and a new modification of [W2(CO)7Br4] ( 3a) were determined by single-crystal X-ray diffraction analysis.
- Subjects
TUNGSTEN; LIGANDS (Chemistry); MOLECULAR structure; X-ray diffraction; CRYSTAL structure
- Publication
Zeitschrift für Anorganische und Allgemeine Chemie, 2013, Vol 639, Issue 8/9, p1559
- ISSN
0044-2313
- Publication type
Article
- DOI
10.1002/zaac.201300036