Abstract
High-temperature reactions of Mo, chalcogen (S or Se), Te, and Br2 in molar ratio Mo: S/Se: Te: Br = 3: 1: 6: 4 were carried out. The reaction products were subjected to mechanochemical activation with K(Dtp) (Dtp = (EtO)2PS2) in a vibrational mill, resulting in the formation of new compounds [Mo3(μ3-Q)0.5(μ3-O)0.5(μ2-Te2)3(Dtp)3](Dtp) (Q = Se (I) and S (II)). The structure of compound I has been established by X-ray diffraction analysis. Solutions of compounds I and II contain mixtures of [Mo3(μ3-Q)(μ2-Te2)3(Dtp)3]+ and [Mo3(μ3-O)(μ2-Te2)3(Dtp)3]+, which is confirmed by mass spectrometry and 31P, 77Se, and 125Te NMR spectroscopy. Quantum-chemical calculations of the 125Te NMR chemical shifts were performed. The compounds are also characterized by IR spectroscopy, Raman spectroscopy, and elemental analysis. Structure I contains short nonvalent contacts between the sulfur atom of the out-of-sphere Dtp anion and the axial tellurium atoms of the cluster.
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