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首页> 外文期刊>Chemistry: A European journal >X-ray Diffraction and Solid-State NMR Studies of a Germanium Binuclear Complex
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X-ray Diffraction and Solid-State NMR Studies of a Germanium Binuclear Complex

机译：锗双核配合物的X射线衍射和固态NMR研究

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摘要

A compound formulated as (C_4H_(12)N_2)[Ge_2(pmida)_2(OH)_2]_4H_2O (where pmida~(4-) = N-(phosphonometh-yl)iminodiacetate and C_4H_(12)N_2~(2+)=pi-perazinedium cation),containing the anionic [Ge_2(pmida)_2(OH)_2]~(2-) complex,has been synthesised by the hydrother-mal approach and its structure determined by single-crystal X-ray diffraction analysis.Several high-resolution solid-state magic-angle spinning (MAS) NMR techniques,in particular two-dimensional ~1H-X(~(13)C,~(31)P) heteronuclear correlation (HETCOR) and ~1H-~1H ho-monuclear correlation (HOMCOR) experiments incorporating a frequency-switched Lee-Goldburg (FS-LG) decoupling scheme,have been employed for the first time in such a material.Using these tools in tandem affords an excellent general approach to study the structure of other inorganic-organic hybrids.We assigned the NMR resonances with the help of C...H and P...H internuclear distances obtained through systematic statistical analyses of the crystallographic data.The compound was further characterised by powder X-ray diffraction techniques,IR and Raman spectroscopy,and by elemental and thermal analyses (thermogravimet-ric analysis and differential scanning calorimetry).
机译：配制为（C_4H_（12）N_2）[Ge_2（pmida）_2（OH）_2] _4H_2O的化合物（其中pmida〜（4-）= N-（膦酰基甲基）亚氨基二乙酸酯和C_4H_（12）N_2〜（2+ ）= pi-perazinedium阳离子），含有阴离子[Ge_2（pmida）_2（OH）_2]〜（2-）配合物，通过水热法合成，其结构通过单晶X射线衍射确定几种高分辨率固态幻角旋转（MAS）NMR技术，尤其是二维〜1H-X（〜（13）C，〜（31）P）异核相关（HETCOR）和〜1H-结合频率切换Lee-Goldburg（FS-LG）去耦方案的〜1H全核相关（HOMCOR）实验已首次在此类材料中使用。串联使用这些工具提供了一种极好的通用研究方法我们通过对晶体学数据进行系统统计分析获得的C ... H和P ... H核间距来分配NMR共振。通过粉末X射线衍射技术，IR和拉曼光谱法以及元素和热分析（热重分析和差示扫描量热法）进一步表征了磅。

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