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Synthesis and Reactivity of the Metallaborane Complex [Mo(CO)4B3H8]- and the Formation of Mo(CO)4(dppe)

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Craig M. Davis and Megan F. Klein

Department of Chemistry, Xavier University, Cincinnati, OH 45207-4221

J. Chem. Educ., 2001, 78 (7), p 952

DOI: 10.1021/ed078p952

Publication Date (Web): July 1, 2001

Abstract

In this laboratory exercise the octahydrotriborate anion ([B₃H₈]^-) is synthesized from sodium borohydride (NaBH₄) and iodine in diglyme under a nitrogen atmosphere, and the sodium salt is converted to the tetrabutylammonium salt by a simple metathesis. Next, the metallaborane complex [(CO)₄MoB₃H₈]^- is prepared by refluxing a solution of Mo(CO)₆ and (Bu₄N)B₃H₈ in anhydrous 1,2-dimethoxyethane (glyme) under a nitrogen atmosphere. This solution is transferred via cannula to a flask containing the solid 1,2-bis(diphenylphosphino)ethane (dppe). The ensuing formation of [Mo(CO)₄(dppe)] is nearly instantaneous. The syntheses of the two metal complexes proceed in very high yield.This exercise features inert-atmosphere syntheses and multinuclear (¹H, ¹¹B, and ³¹P) NMR spectroscopy and is suitable for upper-level undergraduates. The skills and ideas that are taught or reinforced include a general overview of borane clusters and the isolobal analogy, handling air-sensitive solutions, and internuclear coupling in NMR spectra.

Keywords (Audience):

Second-Year Undergraduate

Keywords (Domain):

Inorganic Chemistry

Keywords (Pedagogy):

Hands-On Learning / Manipulatives

Keywords (Subject):

Coordination Compounds

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This article has been cited by 1 ACS Journal articles (1 most recent appear below).

Photochemical Synthesis and Ligand Exchange Reactions of Ru(CO)4(n2-alkene) Compounds
Jason Cooke , David E. Berry and Kelli L. Fawkes
Journal of Chemical Education2007 84 (1), 115
- Photochemical Synthesis and Ligand Exchange Reactions of Ru(CO)4(n2-alkene) Compounds
  Jason Cooke , David E. Berry and Kelli L. Fawkes
  Journal of Chemical Education2007 84 (1), 115
  Irradiation of Ru3(CO)12 in the presence of either methyl acrylate (CH2=CHCO2CH3) or ethylene generates labile Ru(CO)4(η²-alkene) species that readily react with other two-electron donor ligands, such as triphenylphosphine or the more π-acidic alkene ...
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