Structural diversity in molybdenum(VI) complexes with hydrazone-based ligands

U okviru ovog diplomskog rada ispitani su uvjeti nastajanja kompleksa molibdena(VI) s derivatima nikotinhidrazida koji sadrže O i N donorne atome. Provedene su reakcije N'-(2- hidroksi-3-metoksibenziliden)nikotinhidrazona (H2VanNH) i N'-(2-hidroksi-4- metoksibenziliden)nikotinhidrazona (H24OMeSalNH) sa spojevima molibdena(VI), bis(pentan-2,4-dionato)dioksomolibdenom(VI) ([MoO2(acac)2]) i diklorodioksomolibdenom(VI) ([MoO2Cl2]). Reakcije su provedene u metanolu pri različitim temperaturama te su dobiveni kompleksi [MoO2(HVanNH)(MeOH)]Cl, [MoO2(HVanNH)Cl], [MoO2(H4OMeSalNH)Cl] i [MoO2(4OMeSalNH)(MeOH)] (α forma). Reakcijom [MoO2(HVanNH)Cl] s Et3N priređen je koordinacijski polimer [MoO2(VanNH)]n, a deprotonacijom [MoO2(H4OMeSalNH)Cl] je dobiven mononuklearni kompleks [MoO2(4OMeSalNH)(MeOH)] (β forma). Reakcija provedena u solvotermalnim uvjetima pri 110 °C rezultirala je nastajanje polinuklearnog spoja [MoO2(4OMeSalNH)]n. Dobiveni produkti okarakterizirani su na osnovi podataka IR spektroskopije, klasične kemijske analize i termičke analize. Postojanje samo jedne faze potvrđeno je usporedbom difraktograma praha.In this Diploma thesis the synthesis conditions and formation of molybdenum(VI) complexes with nicotinic hydrazide derivatives containing O and N donor atoms were investigated. Reactions of N'-(2-hydroxy-3-methoxybenzilidene)nicotinhydrazone (H2VanNH) and N'-(2-hydroxy-4- methoxybenzilidene)nicotinhydrazone (H24OMeSalNH) with molybdenum(VI) compounds bis(pentane-2,4-dionato)dioxomolybdenum(VI) ([MoO2(acac)2]) and dichlorodioxomolybdenum(VI) ([MoO2Cl2]) were carried out. Complexes [MoO2(HVanNH)(MeOH)]Cl, [MoO2(HVanNH)Cl], [MoO2(H4OMeSalNH)Cl] and [MoO2(4OMeSalNH)(MeOH)] (α form) were obtained when reactions were carried out in methanol at various temperatures,. The coordination polymer [MoO2(VanNH)]n was prepared upon reaction [MoO2(HVanNH)Cl] with Et3N, whereas the mononuclear complex [MoO2(4OMeSalNH)(MeOH)] (β form) was prepared by deprotonation of [MoO2(H4OMeSalNH)Cl]. This reaction performed under solvothermal conditions at 110 °C yielded the polynuclear [MoO2(4OMeSalNH)]n complex. The obtained complexes were characterized by IR spectroscopy, chemical analysis and thermal analysis. The existance of only one phase was confirmed by comparison of the PXRD patterns