Priprava kompleksnih spojeva molibdena i njihova primjena kao katalizatora u reakcijama oksidacije

Synthesis of the dioxomolybdenum(VI) was carried out by using [MoO2(acac)2] and the corresponding ONO hydrazone ligand (2,3-dihydroxbenzaldehyde isonicotinoylhydrazone, H2L1 or 2,3-dihydroxbenzaldehyde nicotinoylhydrazone, H2L2). Polynuclear complexes, [MoO2(L1)]n∙MeCN and [MoO2(L2)]n were obtained from acetonitrile, whereas mononuclear complexes [MoO2(L1,2)(MeOH)] were isolated from methanolic solution. The mechanochemical synthesis employing liquid assisted grinding was also applied, and H2L1 ligand and mononuclear complexes were obtained in such a way. Ex-situ powder X-ray diffraction method was implemented for monitoring H2L1 ligand obtained by mechanochemical synthesis. Complexes were characterized by IR spectroscopy, elemental and termogravimetric analysis. Additionally, polynuclear complexes were characterized by NMR spectroscopy. Molecular and crystal structures of H2L1 ligand and its mononuclear complex were determined by the single crystal X-ray diffraction. Lastly, the complexes were tested as catalyst in oxidation reactions of secondary alcohols, carveol and cyclohexanol by using H2O2 and TBHP (in aqueos solution or solution in decane).U okviru ovog diplomskog rada pripravljeni su molibdenski(VI) kompleksi reakcijom [MoO2(acac)2] i odgovarajućeg hidrazonskog liganda (2,3-dihidroksibenzaldehid izonikotinhidrazona, H2L1 ili 2,3-dihidroksibenzaldehid nikotinhidrazona, H2L2). Izolirani su polinuklearni [MoO2(L1)]n∙MeCN i [MoO2(L2)]n iz acetonitrila i mononuklearni kompleksi [MoO2(L1,2)(MeOH)] iz metanola. Ligand H2L1 i mononuklearne komplekse bilo je moguće sintetizirati mehanokemijski, mljevenjem potpomognuto kapljevinom. Osim toga, mehanokemijska sinteza liganda H2L1 je popraćena ex-situ metodom rentgenske difrakcije na polikristalnom uzorku. Kompleksi su identificirani IR spektroskopijom, elementnom i termogravimetrijskom analizom. Polinuklearni kompleksi karakterizirani su NMR spektroskopijom. Difrakcijom rentgenskog zračenja na monokristalnom uzorku je odreĎena kristalna struktura H2L1 liganda te njegovog mononuklearnog kompleksa. Na kraju, pripravljeni kompleksi su ispitani kao katalizatori u reakcijama oksidacije sekundarnih alkohola, karveola i cikloheksanola u prisutnosti H2O2 i TBHP-a (u vodenoj otopini i otopini u dekanu)