阴离子识别一直以来是超分子领域的研究热点之一。阴离子在生物体中的重要性，使得关于阴离子的结合、识别以及自组装的研究成为一大热点。设计合成不同的阴离子受体与各种阴离子进行识别并研究它们的配位情况至关重要。本文进行了三种多脲受体L¹-L³的设计与合成及其对含氧酸根阴离子的识别性能研究。主要内容如下：
1.三脲受体L¹对有机膦酸根阴离子的识别
以邻苯二胺和1-萘基异氰酸酯为反应原料，合成得到了三脲受体L¹。通过单晶培养条件优化，使用异丙醚扩散法得到了配合物(L¹)(PPA)(TMA)₂以及(L¹)(PPrA)(TPA)₂的单晶结构。单晶结果表明，L¹对有机膦酸根阴离子苯膦酸根(PPA²¯)和膦酸苯酯根(PPrA²¯)均以6条氢键以1:1结合。此外，通过单晶衍射、核磁滴定、高分辨质谱以及荧光滴定研究了L¹对PPA²¯和PPrA²¯的识别性能。结果证明，L¹与PPA²¯和PPrA²¯均形成A₁L₁(A=阴离子，L=配体)的稳定结构，且对PPrA²¯的结合强于PPA²¯，这一结果不受阳离子以及溶剂含水量的影响。
2.四脲受体L²对有机膦酸根阴离子的识别
以邻苯二胺和1-萘基异氰酸酯为反应原料，合成得到了四脲受体L²，研究了L²对PPA²¯和PPrA²¯的识别。通过单晶培养优化，使用异丙醚扩散法得到了配合物(L²)(PPA)(TEA)₂以及(L²)(PPrA)(TPA)₂的单晶。单晶结果表明，L²对PPA²¯和PPrA²¯均以8条氢键以1:1结合。并且通过单晶衍射、核磁滴定、高分辨质谱以及荧光滴定等手段证明了L²与PPA²¯和PPrA²¯的结合比均为1:1，且对PPrA²¯的结合强于PPA²¯，阳离子以及溶剂含水量不影响此结果。
3.吡啶单脲受体L³对醋酸根阴离子的识别
设计合成了间氯苯修饰的吡啶单脲受体L3,并得到了配合物[CuL³(OAc)₂]₂·2AcOH。通过单晶培养优化，使用溶剂浓缩法，得到了L³和配合物[CuL³(OAc)₂]₂·2AcOH的单晶。单晶结构表明，配体L³通过N_脲–H···N_吡啶相互作用和C–H···O相互作用形成二维无限氢键网络，配合物[CuL³(OAc)₂]₂·2AcOH形成由C–H···O氢键延伸的无限氢键链，氢键链结构通过弱的碳氢键相互作用进一步扩展。通过单晶衍射、紫外滴定以及变温磁化率测量确定了A₁L₁结构和反铁磁耦合的特性。

~Anion recognition has always been one of the research hotspots in the field of supramolecules. The importance of anions in organisms makes the research on anion binding, recognition and self-assembly become a hot topic. It is very important to design and synthesize different anion receptors to recognize various anions and to study their coordination. This article discusses the design and synthesis of three polyurea receptors L¹-L³ and their recognition performance for oxyacid anions. The main contents are as follows:
1.Recognition of organophosphonate anions by triurea receptor L¹
Using o-phenylenediamine and 1-naphthyl isocyanate as raw materials, triurea receptor L¹ was synthesized. Through the optimization of single crystal culture conditions, the single crystal structures of complexes (L¹)(PPA)(TMA)₂ and (L¹)(PPrA)(TPA)₂ were obtained using the isopropyl ether diffusion method. The single crystal results show that the L¹ pair of organic phosphonate anion phenylphosphonate (PPA²¯) and phenylphosphonate (PPrA²¯) are both combined 1:1 by 6 hydrogen bonds. In addition, the recognition performance of L¹ to PPA²¯ and PPrA²¯ was studied by single crystal diffraction, nuclear magnetic titration, high-resolution mass spectrometry and fluorescence titration. The results prove that L¹ and PPA²¯ and PPrA²¯ both form a stable structure of A₁L₁ (A=anion, L=ligand), and the binding to PPrA²¯ is stronger than PPA²¯, and the results were not affected by cation and water content of solvent.
2. Recognition of tetraurea receptor L² to organophosphonate anion
Using o-phenylenediamine and 1-naphthyl isocyanate as raw materials, tetraurea receptor L² was synthesized, and the recognition of PPA²¯ and PPrA²¯ by L² was studied. Through the optimization of single crystal culture, single crystals of complexes (L²)(PPA)(TEA)₂ and (L²)(PPrA)(TPA)₂ were obtained using isopropyl ether diffusion method. The single crystal results show that L² binds PPA²¯ and PPrA²¯ at a 1:1 ratio with 8 hydrogen bonds. And through single crystal diffraction, nuclear magnetic titration, high-resolution mass spectrometry and fluorescence titration, it is proved that the binding ratio of L² to PPA²¯ and PPrA²¯ is 1:1, and the binding of PPrA²¯ is stronger than that of PPA²¯. The cation and solvent contain The amount of water does not affect this result.
3. Recognition of acetate anion by pyridine monourea receptor L³
M-chlorobenzene modified pyridine monourea receptor L³ was designed and synthesized, and the complex [CuL³(OAc)₂]₂·2AcOH was obtained. Through the optimization of single crystal culture and the solvent concentration method, single crystals of L³ and the complex [CuL³(OAc)₂]₂·2AcOH were obtained. The single crystal structure shows that the ligand L³ forms a two-dimensional infinite hydrogen bond network through the interaction of N_urea−H···N_pyridine and the interaction of C−H···O. The complex [CuL³(OAc)₂]₂·2AcOH forms an infinite hydrogen bond chain extended by C−H···O hydrogen bonds, and the hydrogen bond chain structure is further expanded by weak carbon-hydrogen bond interactions. The characteristics of A₁L₁ structure and antiferromagnetic coupling were determined by single crystal diffraction, ultraviolet titration, and temperature-varying magnetic susceptibility measurement.

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