Abstract

The reaction of [Mo₃S₄(Tu)₈(H₂O)]Cl₄·4H₂O (Tu is thiourea) with (PhCH₂CH₂)₂-PCH₂CH₂SeC₅H₁₁) (PSe) followed by purification on a chromatographic column packed with silica gel using a saturated solution of KPF₆ in acetone as an eluent results in the formation of [Mo₃S₄Cl₃(PSe)₃]PF₆ (I) in a yield of 44%. Compound I is characterized by X-ray diffraction analysis, ¹H, ³¹P{¹H}, and ⁷⁷Se NMR spectroscopy, IR spectroscopy, UV-Vis spectroscopy, cyclic voltammetry, and electrospray ionization mass spectrometry. Several species differed in the coordination mode of three PSe ligands, which can bind to molybdenum via one (phosphorus) or two (phosphorus and selenium) donor atoms, are formed in a solution of compound I at room temperature. This behavior is not observed for the compounds similar in structure with PS ligands of an analogous type. Complex I demonstrates a higher catalytic activity than its analogue with the PS ligand in the reduction of nitrobenzene to aniline under the action of diphenylsilane.

中文翻译：

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具有半不稳定的膦-硒醚配体的新型簇络合物{Mo 3 S 4}的合成与表征

摘要

[Mo ₃ S ₄（Tu）₈（H ₂ O）] Cl ₄ ·4H ₂ O（Tu是硫脲）与（PhCH ₂ CH ₂）₂ -PCH ₂ CH ₂ SeC ₅ H ₁₁）（PSe）的反应然后在装有硅胶的色谱柱上纯化，使用KPF ₆在丙酮中的饱和溶液作为洗脱液，可以形成[Mo ₃ S ₄ Cl ₃（PSe）₃ ] PF ₆（I），产率为44 ％。化合物IX射线衍射分析，¹ H，³¹ P { ¹ H}和⁷⁷ Se NMR光谱，IR光谱，UV-Vis光谱，循环伏安法和电喷雾电离质谱法的表征。在室温下，在化合物I的溶液中形成了三个PSe配体的配位模式不同，这三个PSe配体可以通过一个（磷）或两个（磷和硒）供体原子与钼结合。对于在结构上与类似类型的PS配体相似的化合物，未观察到此行为。复杂的我 在二苯硅烷的作用下，证明硝基苯还原为苯胺比其具有PS配体的类似物具有更高的催化活性。