Variable-temperature 13C solid-state NMR spectra: Mobility of trimethyltin groups in coordination polymers of the type [(Me3Sn)4M(CN)6]∞ (MFe, Os, Ru)

Robin K. Harris, M.Maral Sünnetçioğlu , R.Dieter Fischer
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引用次数: 12

Abstract

Solid-state 13C CP MAS NMR studies of compounds [(Me3Sn)4M(CN)6]∞ with MFe, Ru and Os were performed over a temperature range of 80 K in order to understand exchange thermodynamics. For each compound six methyl carbon signals are seen below 240 K, showing there are two non-equivalent Me3Sn units. Using detailed lineshape analysis the thermodynamic activation parameters for the three samples were obtained. Low-temperature 2-D exchange spectra indicated that exchange occurs between the carbons of each Me3Sn rotor independently. Therefore in the calculations a model of two independent three-site mutual-exchange processes was used. The effect of 117/119Sn satellites was included.

[(Me3Sn)4M(CN)6]∞(MFe, Os, Ru)型配位聚合物中三甲基锡基团的迁移率
为了了解交换热力学,在80 K的温度范围内对含有MFe、Ru和Os的化合物[(Me3Sn)4M(CN)6]∞进行了固态13C CP MAS NMR研究。对于每个化合物,在240 K以下可以看到6个甲基碳信号,表明存在两个不等效的Me3Sn单元。通过详细的线形分析,得到了三种样品的热力学活化参数。低温二维交换光谱表明,Me3Sn转子各碳原子之间的交换是独立发生的。因此,在计算中采用了两个独立的三位点相互交换过程模型。考虑了117/119Sn卫星的影响。
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