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The novel dioxomolybdenum(VI) complexes with methyl (1), ethyl (2), n-propyl (3), i-propyl (4), n-butyl (5) and cyclohexyl (6) ester of 2-mercaptonicotinic acid have been prepared in the reactions of MoO 2 Cl 2 and MoO 2 -(acac) 2 (acac = 2,4-pentandionate) with mercaptonicotinic acid in corresponding alcohol. The esterification reaction was catalyzed by Mo V originated from the reduction of Mo VI with mercaptonicotinic -SH group with simultaneous formation of S±S bond resulting from the condensation of two 2-mercaptonicotinic molecules. The presence of Mo V was proved by ESR spectra. The molecular and crystal structures of 1, 2, 3 and 4 as well as of the by-products 1,1'-dithio-2,2'-n-butylnicotinoate (7) and tetramethylammonium hexachloromolybdate(V) (8) have been determined by a X-ray single crystal diffraction. The complexes 1±4 contain MoO 2 2+ core with octahedral coordination of each molybdenum atom complexed by two 2-mercaptonicotinato N and S donor atoms.

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