Improved syntheses of [Cp2* Mo2 O5] and [Cp2* W2 O5]: Structural characterization of Na[Cp*MoO3] · 5H2O and [Cp2* W2 O5]

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Dinoi C., Taban G., AKTAŞ P., DEMİRHAN F., Daran J., Poli R.

Journal of Organometallic Chemistry, vol.692, no.17, pp.3743-3749, 2007 (SCI-Expanded, Scopus) identifier identifier

  • Publication Type: Article / Article
  • Volume: 692 Issue: 17
  • Publication Date: 2007
  • Doi Number: 10.1016/j.jorganchem.2007.05.021
  • Journal Name: Journal of Organometallic Chemistry
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Page Numbers: pp.3743-3749
  • Keywords: molybdenum, tungsten, aqueous organometallic chemistry, oxo ligands, pentamethylcyclopentadienyl ligands
  • Open Archive Collection: AVESIS Open Access Collection
  • Manisa Celal Bayar University Affiliated: Yes

Abstract

Use of aqueous conditions and the ROOH (R = tBu or H) compounds as oxidizing agents affords a simple two-step, one-pot synthetic procedure leading to [Cp2* M2 O5] (M = Mo, W) from [M(CO)6] selectively and in high yields. The hexacarbonyl compounds are converted to Na[Cp*M(CO)3] in refluxing THF, then the mixture is diluted with water (W) or aqueous NaOH (Mo) and directly treated with 6 equiv. of ROOH. Acidification of an aqueous solution of the Na[Cp*MO3] product affords spectroscopically pure [Cp2* M2 O5] in high isolated yields (global yields from [M(CO)6], for R = tBu: Mo, 91%; W, 87%). The X-ray structures of Na[Cp*MoO3] · 5H2O and [Cp2* W2 O5] are also reported. © 2007 Elsevier B.V. All rights reserved.