ISSN:
1572-8862
Keywords:
deprotonated amines
;
sulfur-bridge
;
incomplete cubane-type
;
molybdenum cluster
;
1H NMR
Source:
Springer Online Journal Archives 1860-2000
Topics:
Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
,
Physics
Notes:
Abstract Oxygen/sulfur-bridged incomplete cubane-type molybdenum aqua clusters [Mo3(μ 3-S)(μ-X)(μ-S)2(H2O)9]4+ (X=O, S) in hydrochloric acid react with dien (diethylenetriamine) to give [Mo3(μ 3-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−], respectively, where each cluster has a deprotonated dien. The X-ray structural analysis of 1 revealed proton dissociation from an amino group of one of the three dien ligands: one Mo–N distance [1.987(4) Å] is clearly shorter than the other eight Mo–N distances [2.229(3)–2.276(3) Å]. 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 dissociation are discussed.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1023/A:1009045722437
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