Cu(II) and Mo(VI) complexes with selected (thio)carbonohydrazides

Cilj ovog rada bio je pripraviti mješovite kompleksne spojeve molibdena(VI) i bakra(II) sa simetričnim disupstituiranim (tio)karbonohidrazidima priređenih iz 2-hidroksibenzaldehida ili 2-hidroksi-3-metoksibenzaldehida. U oviru rada također su pripravljeni mono-, di- i polinuklearni kompleksni spojevi molibdena(VI) te mono- i dinuklearni kompleksni spojevi bakra(II). Sinteze su provedene u otopinama metanola, acetona i acetonitrila, dok su neki od spojeva pripravljeni i mehanokemijski. Analiza i identifikacija pripravljenih spojeva provedene su metodama infracrvene spektroskopije, nuklearne magnetske rezonancije, termogravimetrije, razlikovne pretražne kalorimetrije i rentgenske difrakcije na polikristalnom uzorku. Spektroskopijom nuklearne magnetske rezonancije potvrđene su molekulske strukture triju kompleksnih spojeva ([MoO2(H2T3OMe)]2, [MoO2(H2T)]n i [MoO2(H2T)(MeOH)]) te jednog od četiri korištena liganda 1,5-bis(2-hidroksibenziliden)tiokarbonohidrazida (H4T). Nadalje, prekristalizacijom kompleksnog spoja [MoO2(H2T)(MeOH)] u etanolu, dobiven je jedinični kristal te je difrakcijom rentgenskog zračenja na jediničnom kristalu određena molekulska i kristalna struktura kompleksnog spoja [MoO2(H2T)(EtOH)][MoO2(H2T)(H2O)]×EtOH.The aim of this research was the preparation and structural characterization of heteronuclear molybdenum(VI) and copper(II) complexes with symmetrical disubstituted (thio)carbohydrazides derived from 2-hydroxybenzaldehyde or 2-hydroxy-3-methoxybenzaldehyde. Furthermore, mono-, di- and polynuclear complexes of molybdenum(VI) and mono- and dinuclear complexes of copper(II) were prepared. Complexes were synthesized from solutions (methanol, acetonitrile, and acetone), while some complexes were also prepared mechanochemically. All compounds were identified by the infrared spectroscopy, nuclear magnetic resonance, thermogravimetric analysis, differential scanning calorimetry, and powder X-Ray diffraction. Molecular structures of complexes [MoO2(H2T3OMe)]2, [MoO2(H2T)]n, [MoO2(H2T)(MeOH)] and ligand 1,5-bis(2-hydroxybenzaldehyde)thiocarbohydrazone (H4T) were determined by nuclear magnetic resonance spectroscopy. Recrystallization of the synthesized mononuclear complex [MoO2(H2T)(MeOH)] in ethanol resulted in the formation of single-crystal whose molecular and crystal structure was determined by the single-crystal X-ray diffractio