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Issue 12, 2014
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Dioxomolybdenum(vi) and dioxotungsten(vi) complexes chelated with the ONO tridentate hydrazone ligand: synthesis, structure and catalytic epoxidation activity

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Abstract

Synthesis of the dioxomolybdenum(VI) complexes [MoO2(L3OMe)(EtOH)] (1), [MoO2(L4OMe)(EtOH)] (2) and [MoO2(LH)(EtOH)] (3) and dioxotungsten(VI) complexes [WO2(L3OMe)(EtOH)] (4), [WO2(L4OMe)(EtOH)] (5) and [WO2(LH)]n (6a) was carried out using [MO2(C5H7O2)2] (M = Mo or W) and the corresponding aroylhydrazone ligand H2LR (3-methoxysalicylaldehyde 4-hydroxybenzhydrazone (H2L3OMe), 4-methoxysalicylaldehyde 4-hydroxybenzhydrazone (H2L4OMe), or salicylaldehyde 4-hydroxybenzhydrazone (H2LH) in ethanol. Compounds obtained upon heating of the mononuclear complexes in acetonitrile or dichloromethane, [MO2(LR)]n (1a–6a) or [MoO2(L3OMe)]2 (1b), respectively, were also investigated. Crystal and molecular structures of the mononuclear 1, 2 and 3, polynuclear 1a·MeCN and dinuclear 1b complexes were determined by the single crystal X-ray diffraction method. Powder X-ray diffraction showed isostructurality of 1 and 4, and 2 and 5. The complexes were further characterized by elemental analysis, IR spectroscopy, TG and DSC analyses, and one- and two-dimensional NMR spectroscopy. The catalytic performances of 1–5 and 6a were investigated for epoxidation of cyclooctene using aqueous tert-butyl hydroperoxide (TBHP) as the oxidant.

Graphical abstract: Dioxomolybdenum(vi) and dioxotungsten(vi) complexes chelated with the ONO tridentate hydrazone ligand: synthesis, structure and catalytic epoxidation activity

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Supplementary files

Article information


Submitted
18 Aug 2014
Accepted
06 Oct 2014
First published
06 Oct 2014

New J. Chem., 2014,38, 6176-6185
Article type
Paper

Dioxomolybdenum(VI) and dioxotungsten(VI) complexes chelated with the ONO tridentate hydrazone ligand: synthesis, structure and catalytic epoxidation activity

V. Vrdoljak, J. Pisk, D. Agustin, P. Novak, J. Parlov Vuković and D. Matković-Čalogović, New J. Chem., 2014, 38, 6176
DOI: 10.1039/C4NJ01394H

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