We report 4-methoxysalicylaldhyde S-allyl isothiosemicarbazone (HL) and its Mo(VI) complexes, [ML]. The crystal structure analysis indicates that the metal has six-coordinate distorted octahedral geometry. All experimental results confirmed that HL is a tridentate mono-deprotonated ligand (NNO), coordinating through phenolic oxygen, azomethine nitrogen, and isothioamide nitrogen. MoO2 bond lengths and angles are 1.701(12)-1.719(11) Å and 104.30(7)-105.44(6)˚, respectively. The distances of Mo1-O5 (2.321(1) Å) and Mo1-N4 (2.345(14) Å) for Mo(VI) complexes, are the longest in the coordination sphere of Mo.

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