Publication | Closed Access
Formation and Structural Diversity of Organo‐Functionalized Tin–Silver Selenide Clusters
15
Citations
35
References
2017
Year
When reacting the organic functionalized tin selenide clusters [(SnR<sup>1</sup> )<sub>3</sub> Se<sub>4</sub> Cl] (A, R<sup>1</sup> =CMe<sub>2</sub> CH<sub>2</sub> C(O)Me) or [(SnR<sup>1</sup> )<sub>4</sub> Se<sub>6</sub> ] (B) with (SiMe<sub>3</sub> )<sub>2</sub> Se and [Ag(PPh<sub>3</sub> )<sub>3</sub> Cl] at -78 °C in CH<sub>2</sub> Cl<sub>2</sub> , a microcrystalline intermediate (compound 1) precipitates, which was investigated by magic angle spinning (MAS) NMR spectroscopy, powder X-ray diffraction (PXRD), energy dispersive X-ray (EDX) spectroscopy, and quantum chemistry calculations, to derive information about its composition and structure. Compound 1 re-dissolves under reorganization into the organo-functionalized Ag/Sn/Se cluster compound [Ag<sub>6</sub> (μ<sub>6</sub> -Se)(Ag<sub>8</sub> Se<sub>12</sub> ){(R<sup>1</sup> Sn)<sub>2</sub> Se<sub>2</sub> }<sub>6</sub> ] (2), or the mixed-valence cluster [(AgPPh<sub>3</sub> )<sub>2</sub> (Sn<sup>II</sup> Cl)<sub>2</sub> Se<sub>2</sub> {(R<sup>1</sup> Sn<sup>IV</sup> )<sub>2</sub> Se<sub>2</sub> }<sub>2</sub> ] (3), depending on the presence or the exclusion of daylight, respectively. The addition of N<sub>2</sub> H<sub>4</sub> ⋅H<sub>2</sub> O to a solution of 1 yields selectively [Ag<sub>7</sub> (μ<sub>7</sub> -Se)(Ag<sub>7</sub> Se<sub>12</sub> ){(R<sup>2</sup> Sn)<sub>2</sub> Se<sub>2</sub> }<sub>6</sub> ] (4, R<sup>2</sup> =CMe<sub>2</sub> CH<sub>2</sub> C(N<sub>2</sub> H<sub>2</sub> )Me), the Ag/Sn/Se core of which is isomeric to that of 2. 2-4 were characterized by X-ray diffraction. NMR spectroscopic studies on solutions of 1 indicate the co-existence of different species.
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