Four trinuclear dioxidomolybdenum(VI) complexes, [{Mo VI O 2 (H 2 O)} 3 ptk(bhz) 3 ] (1), [{Mo VI O 2 (H 2 O)} 3 ptk(fah) 3 ] (2), [{Mo VI O 2 (H 2 O)} 3 ptk(inh) 3 ] (3), and [{Mo VI O 2 (H 2 O)} 3 ptk(nah) 3 ] (4), based on the tritopic central 2,4,6-triacetylphloroglucinol (H 3 ptk) ligands H 6 ptk(bhz) 3 (I), H 6 ptk(fah) 3 (II), H 6 ptk(inh) 3 (III) and H 6 ptk(nah) 3 (IV) (Hbhz = benzoylhydrazide, Hfah = 2furanoylhydrazide, Hinh = isonicotinoylhydrazide and Hnah = nicotinoylhydrazide), respectively, are presented. All of the synthesized ligands, as well as their complexes, have been characterized by elemental, thermal, and electrochemical analyses, spectroscopic techniques (FTIR, UV/Vis, 1 H and 13 C NMR), and single-crystal X-ray studies of [{Mo VI O 2 (H 2 O)}{Mo VI O 2 (MeOH)} 2ptk(bhz) 3 ]·2H 2 O·1.25MeOH (1a) and [{Mo VI O 2 (EtOH)} 3 ptk-[a]
2952[a] Total mass loss considering the temperature range given in the previous column.
Binuclear molybdenum(vi) complexes with a μ-O{MoO2}2 core as catalysts for the oxidation of bicyclic alcohols (fenchyl alcohol and isoborneol), using 30% H2O2 as the oxidant in the presence of NEt3 as the additive, are reported.
= 4,6-diacetyl resorcinol and Hbhz = benzoylhydrazide, Hinh = isonicotinoylhydrazide, Hnah = nicotinoylhydrazide, and Hfah = 2-furoylhydrazide) have been prepared by the reaction of ligand with [Mo VI O 2 (acac) 2 ] (Hacac = acetylacetone) in 1:2 ratio in methanol. Isolated complexes(4) are characterized by elemental (CHN) analysis, spectral (FT-IR, UV-vis, 1 H and 13 C NMR) and thermogravimetric analysis.Single crystal X-ray diffraction analysis of complexes 1, 2 and 4 confirms their binuclear structure and distorted octahedral geometry around each molybdenum where ligands behave as bis(dibasic tridentate) coordinating through phenolic oxygen, azomethine nitrogen and enolic oxygen atoms of each unit. These complexes have successfully been used as catalyst precursors in solvent as well as solvent free conditions for the one-pot three components (ethylacetoacetate, benzaldehyde and ammonium acetate) dynamic covalent assembly, via Hantzsch reaction using hydrogen peroxide as an oxidant.
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