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crystal structure molybdenum sulfido oxo diethylenetriaminato trinuclear cluster; molybdenum sulfido oxo diethylenetriaminate trinuclear cluster prepn structure; deprotonation diethylenetriamine molybdenum sulfido oxo trinuclear cluster
Oxygen/sulfur-bridged incomplete cubane-type molybdenum aqua clusters [Mo3(μ3-S)(μ-X)(μ-S)2(H2O)9]4+ (X = O, S) in hydrochloric acid react with dien (diethylenetriamine) to give [Mo3(μ3-S)(μ-X)(μ-S)2(dien-)(dien)2]Cl3.nH2O [1, X = O, n = 3; 2, X = S, n = 4; dien- = NH2(CH2)2NH(CH2)2NH-], resp., where each cluster has a deprotonated dien. The x-ray structural anal. of 1 revealed proton dissocn. from an amino group of one of the three dien ligands: one Mo-N distance [1.987(4) angstrom] is clearly shorter than the other eight Mo-N distances [2.229(3)-2.276(3) angstrom]. The 1H NMR spectra of the Mo-dien clusters 1 and 2 in D2O show two well-resolved methylene proton signals in the 2.8- to 3.0-ppm region, which indicates that both deprotonated amines in 1 and 2 receive D+ ions from solvent D2O. The factors for the proton dissocn. are discussed.
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