Journal
ORGANOMETALLICS
Volume 38, Issue 19, Pages 3719-3729Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.organomet.9b00472
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Funding
- Daimler and Benz Foundation
- Fonds der Chemischen Industrie
- Young Academy of the North Rhine-Westphalian Academy of Sciences, Humanities and the Arts
- University of Paderborn
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We report the facile synthesis of five rare high-valent Mo(VI)-NHC complexes with a dianionic OCO-pincer benzimidazolylidene ligand (L-1) with the general formula (LMoO2)-Mo-1 (1), (LMo)-Mo-1(O)((NBu)-Bu-t)(THF) (2), (LMo)-Mo-1((NBu)-Bu-t)((NHBu)-Bu-t)Cl (3), (LMo)-Mo-1((NBu)-Bu-t)(2) (4), and L-1 Mo(NMes)(2) (5). These complexes represent a complete series of high-valent molybdenum(VI) complexes, obtained by consecutive exchange of the oxo for imido ligands from the dioxo complex (1) to the bis-imido complexes (4 and 5). The complexes can be synthesized in high yields following a simple deprotonation protocol, using either triethylamine or lithium diisopropylamide (LDA) as a base. All complexes have been characterized by various techniques, including H-1, C-13{H-1}, and N-15 NMR spectroscopy, IR spectroscopy, and X-ray diffraction analysis. Except for the dioxo complex 1, all complexes adopt monomeric structures in the solid state. Compounds 1, 4, and 5 are rare examples of five-coordinated molybdenum(VI) complexes in the solid state, while 2 is six-coordinated, having a weakly bound THF ligand in the axial position. The dioxo complex 1 was found to be stable under air and moisture in the solid state as well as in solution for several days. Furthermore, preliminary reactivity studies and an approximate determination of the pK(a) value of the imido ligands in 4 are presented.
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