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First isolated active titanium peroxo complex: characterization and theoretical study.

Oxana A Kholdeeva1, Tatiana A Trubitsina, Raisa I Maksimovskaya

  • 1Boreskov Institute of Catalysis, Pr. Lavrentieva 5, Novosibirsk 630090, Russia.

Inorganic Chemistry
|March 30, 2004
PubMed
Summary
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This study introduces a novel protonated titanium peroxo complex, [Bu(4)N](4)[HPTi(O(2))W(11)O(39)] (1), which exhibits distinct reactivity compared to its unprotonated counterpart. The protonated complex readily oxidizes 2,3,6-trimethylphenol via a homolytic mechanism, yielding different products based on reactant ratios.

Area of Science:

  • Inorganic Chemistry
  • Materials Science
  • Catalysis

Background:

  • Titanium peroxo complexes are crucial in oxidation catalysis.
  • Protonation effects on heteropolytungstates are not fully understood.
  • The synthesis and characterization of novel titanium peroxo complexes are essential for advancing catalytic applications.

Purpose of the Study:

  • To synthesize and characterize a novel protonated titanium peroxo complex, [Bu(4)N](4)[HPTi(O(2))W(11)O(39)] (1).
  • To investigate the structural and electronic properties of the protonated complex and compare them to its unprotonated analog.
  • To explore the reactivity of the protonated complex in the oxidation of 2,3,6-trimethylphenol (TMP) and elucidate the reaction mechanism.

Main Methods:

  • Synthesis of the protonated titanium peroxo complex via reaction of a micro-oxo dimeric heteropolytungstate with hydrogen peroxide.

Related Experiment Videos

  • Characterization using elemental analysis, UV-vis, IR, resonance Raman (RR), 31P and 183W NMR spectroscopy, cyclic voltammetry, and potentiometric titration.
  • Reactivity studies involving the oxidation of TMP, product analysis (BP and TMBQ), and deuterium labeling experiments. DFT calculations were also employed.

    • Main Results:

    • The successful synthesis and characterization of the protonated titanium peroxo complex (1) with a Keggin-type structure and a peroxo ligand coordinated to Ti(IV).
    • Protonation significantly increases the redox potential of the peroxo group and alters NMR spectral features compared to the unprotonated complex (2).
    • Complex 1 readily oxidizes TMP, producing either 2,2',3,3',5,5'-hexamethyl-4,4'-biphenol (BP) or 2,3,5-trimethyl-p-benzoquinone (TMBQ) depending on the reactant ratio, suggesting a homolytic oxidation mechanism involving phenoxyl radicals.

    Conclusions:

    • The protonated titanium peroxo complex (1) is a stable monomeric Keggin-type species with unique electrochemical and reactivity profiles.
    • The protonation site is likely a Ti-O-W bridging oxygen, influencing the complex's catalytic activity.
    • The observed oxidation of TMP proceeds via a homolytic pathway, with product distribution controlled by reactant stoichiometry, highlighting the potential of this complex in selective oxidation reactions.