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首页> 外文期刊>The journal of physical chemistry, C. Nanomaterials and interfaces >Single Crystal Electron Paramagnetic Resonance with Dielectric Resonators of Mononuclear Cu2+ Ions in a Metal-Organic Framework Containing Cu-2 Paddle Wheel Units
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Single Crystal Electron Paramagnetic Resonance with Dielectric Resonators of Mononuclear Cu2+ Ions in a Metal-Organic Framework Containing Cu-2 Paddle Wheel Units

机译：含Cu-2桨轮单元的金属有机骨架中单核Cu2 +离子介电共振器的单晶电子顺磁共振

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摘要

Dielectric resonator aided sensitivity-enhancing electron paramagnetic resonance was successfully applied to small single crystals of the previously reported metal-organic framework compound (3)(infinity)[(Cu2Cu2II)-Cu-I(H2O)(2)L2Cl2] in a conventional X-band EPR spectrometer at 7 K sample temperature to reveal the nature of mononuclear Cu2+ ion defect species. We found that these paramagnetic defects are not related to an impurity phase or extraframework species of the parent metal organic framework material but are formed within the framework. Novel angular resolved single crystal continuous wave electron paramagnetic resonance supported by powder measurements and single crystal X-ray diffraction on this metal organic framework compound identified defective copper paddle wheel units with one missing Cu2+ ion as the observed mononuclear paramagnetic species in this compound. The sensitivity enhancement by an estimated factor of 8.6 for the single crystal electron paramagnetic resonance spectroscopy is required to efficiently record the Cu2+ ion signals in single crystals of typical sizes of 200 x 50 x 50 mu m(3) at X-band frequencies. The results demonstrate that conventional electron paramagnetic resonance spectrometers operating at X-band frequencies and equipped with dielectric resonators can successfully be used to perform single crystal studies of these porous, low density materials with very small volume samples at low temperatures.
机译：在常规方法中，介电共振器辅助灵敏度增强电子顺磁共振已成功应用于先前报道的金属-有机骨架化合物（3）（无穷大）[（Cu2Cu2II）-Cu-I（H2O）（2）L2Cl2]的小单晶X波段EPR光谱仪在7 K的样品温度下揭示了单核Cu2 +离子缺陷物种的性质。我们发现这些顺磁缺陷与母体金属有机骨架材料的杂质相或骨架外物种无关，而是在骨架内形成的。在该金属有机骨架化合物上进行粉末测量和单晶X射线衍射所支持的新型角分辨单晶连续波电子顺磁共振，鉴定出具有一个缺失的Cu2 +离子的有缺陷的铜桨轮单元，作为该化合物中观察到的单核顺磁物质。为了在X波段频率下有效记录200 x 50 x 50μm（3）典型尺寸的单晶中的Cu2 +离子信号，需要单晶电子顺磁共振波谱的灵敏度提高8.6倍。结果表明，在X波段频率下运行并配备介电共振器的常规电子顺磁共振波谱仪可成功地用于对这些多孔，低密度材料进行少量体积的低温单晶研究。

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