Intercalation of (η5-Pentamethylcyclopentadienyl)trioxomolybdenum(VI) in a Layered Double Hydroxide

Ana C. Gomes, Patrícia Neves, Sandra Gago, Anabela A. Valente, Isabel S. Gonçalves, Martyn Pillinger

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Abstract

A Zn,Al layered double hydroxide (LDH) with [Cp*MoO3] (Cp* = η5-C5Me5) anions in the interlayer has been prepared by a direct coprecipitation method. The intercalated LDH and the mixed metal oxide (MMO) obtained after its calcination were characterized by elemental and thermogravimetric analyses, powder X-ray diffraction (PXRD), FT-IR and FT-Raman spectroscopy, 13C and 27Al MAS NMR, and scanning electron microscopy. The observed basal spacing of 17.1 Å for the LDH Zn,Al-Cp*MoO3 (corresponding to a gallery height of 12.3 Å) suggests that the guest anions self-assemble into dimers via offset face-to-face Cp*···Cp* interactions, which facilitates hydrogen-bonding interactions between the oxido ligands of the complexes and the layer hydroxyl groups, while positioning the hydrophobic aromatic rings towards the center of the galleries. Calcination of Zn,Al-Cp*MoO3 at 550 °C under air gave an MMO comprising well-dispersed ZnO, α-ZnMoO4 and ZnAl2O4 (spinel) oxides in a molar of ca. 1.4:1.6:1. The MMO exhibited catalytic activity for the epoxidation of cis-cyclooctene with tert-butylhydroperoxide (TBHP) as terminal oxidant, with quantitative yield of the epoxide being achieved within 24 h at 85 °C.

Original languageEnglish
Pages (from-to)2408-2416
Number of pages9
JournalEuropean Journal of Inorganic Chemistry
Volume2020
Issue number25
DOIs
Publication statusPublished - 7 Jul 2020

Keywords

  • Cyclopentadienyl ligands
  • Half-sandwich complexes
  • Layered compounds
  • Molybdenum
  • Oxido ligands

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