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Molybdenum complexes with organic thiolic ligands have drawn the attention of both chemists and biologists for more than four decades because of their potential applications for inorganic models of active centers of molybdenum enzymes, such as xanthine oxidase, sulfite oxidase, and DMSO reductase.1–3 Recently we reported on a dinuclear molybdenum complex with 2-(2-aminoethyl)aminoethanethiol (Haeaet).4 As an extension of this work, we tried to obtain a new molybdenum complex by using 2-(3-aminopropyl)aminoethanethiol (Hapaet), which is a similar ligand to Haeaet, but different in the methylene length. So far, mono-, di-, tri-, tetra-, hexa-, octa-, and polynuclear complexes have been isolated for the Hapaet and related ligands.5–17 In this study, we isolated a trinuclear molybdenum complex with apaet–, [Mo3O7(apaet)2] (1) as single crystals, and determined the crystal structure, as shown in Fig. 1. [Mo3O7(apaet)2]·2CH3OH (1·2CH3OH): Synthesis was carried out by the standard Schlenk techniques under argon. The Hapaet was synthesized by a procedure described in the literature.5 To a methanol solution (10 cm3) of Hapaet (49.6 mg, 0.369 mmol) was added a solution of methanol (10 cm3) containing a small amount (0.2 cm3) of dimethyl sulfoxide of dioxidobis(acetylacetonato)molybdenum(VI) (58.8 mg, 0.180 mmol); the mixed solution was then stirred for a while. The resulting brown solution was filtered and the filtrate was left standing for several days to give brown crystals. 2018 © The Japan Society for Analytical Chemistry

x-ray structure analysis online

Synthesis, Crystal Structure, and Relativistic DV-Xα Calculation of a μ-Oxido-μ-molybdato(VI)-bridged Dinuclear Oxidomolybdenum(V) Complex with 2-(3-Aminopropyl)aminoethanethiol