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.