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Construction of Four Copper Coordination Polymers Derived from a Tetra-Pyridyl-Functionalized Calix[4]arene: Synthesis, Structural Diversity, and Catalytic Applications in the A3 (Aldehyde, Alkyne, and Amine) Coupling Reaction
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2017-09-08 00:00:00 , DOI: 10.1021/acs.cgd.7b00898 Cai-Xia Yu 1 , Fei-Long Hu 2 , Meng-Yu Liu 1 , Cai-Wen Zhang 1 , Yun-He Lv 1 , Shu-Kuan Mao 1 , Lei-Lei Liu 1
Crystal Growth & Design ( IF 3.2 ) Pub Date : 2017-09-08 00:00:00 , DOI: 10.1021/acs.cgd.7b00898 Cai-Xia Yu 1 , Fei-Long Hu 2 , Meng-Yu Liu 1 , Cai-Wen Zhang 1 , Yun-He Lv 1 , Shu-Kuan Mao 1 , Lei-Lei Liu 1
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Solvothermal reactions of CuX2 (X = NO3, Cl, Br, I) with tetra-pyridyl-functionalized calix[4]arene at 130 °C afforded four novel coordination polymers, {[(CuNO3)2L]·MeOH}n (1), [(CuCl2)L0.5]n (2), [(Cu3Br3)L]n (3), and [(Cu3I3)L]n (4), where L = 25,26,27,28-tetra[(3-pyridylmethyl)oxy]calix[4]arene. All the products were characterized by infrared spectroscopy, thermogravimetric analysis, single-crystal X-ray diffraction, and powder X-ray diffraction. Crystal structure analysis reveals that 1 holds a one-dimensional (1D) double-chain constructed by mononuclear [Cu(NO3)] units and L linkers, while 2 features a 1D chain and its bowl-shaped L ligands work as linkers to connect the dinuclear [Cu2Cl4] units. Compounds 3 and 4 bear similar two-dimensional networks, in which each trinuclear [Cu3Br3]/[Cu3I3] unit works as a three-connecting node to connect its six equivalents by sharing L ligands. These results demonstrate that different anions have a significant effect on the final structure formation. Compounds 1–4 were employed as catalysts for the A3 coupling reaction under microwave irradiation. Notably, 3 showed the best catalytic properties for the synthesis of versatile propargylamines (yield up to 94% in only 10 min) from the A3 reaction of formaldehyde with a variety of alkynes and amines.
中文翻译：
四吡啶基官能杯[4]芳烃衍生的四种铜配位聚合物的构建：在A 3（醛，炔和胺）偶联反应中的合成，结构多样性和催化应用
CuX 2（X = NO 3，Cl，Br，I）与四吡啶基官能化杯[4]芳烃在130°C的溶剂热反应制得四种新型配位聚合物，{[（（CuNO 3）2 L]·MeOH} n（1），[（CuCl 2）L 0.5 ] n（2），[（Cu 3 Br 3）L] n（3）和[（Cu 3 I 3）L] n（4），其中L = 25,26,27,28-四[（3-吡啶基甲基）氧基]杯[4]芳烃。所有产品均通过红外光谱，热重分析，单晶X射线衍射和粉末X射线衍射进行表征。晶体结构分析表明，1拥有由单核[Cu（NO 3）]单元和L个连接基构成的一维（1D）双链，而2个具有1D链，其碗形L配体起着连接连接基的作用。双核[Cu 2 Cl 4 ]单元。化合物3和4具有相似的二维网络，其中每个三核[Cu 3 Br 3 ] / [Cu 3 I3 ]单元充当三个连接节点，通过共享L个配体连接其六个等价物。这些结果表明，不同的阴离子对最终结构的形成具有重大影响。化合物1 - 4被用作催化剂为A 3微波辐射下偶联反应。值得注意的是，3显示出甲醛与各种炔烃和胺的A 3反应合成多功能炔丙胺的最佳催化性能（仅10分钟内收率高达94％）。
更新日期：2017-09-08
中文翻译：
四吡啶基官能杯[4]芳烃衍生的四种铜配位聚合物的构建：在A 3（醛，炔和胺）偶联反应中的合成，结构多样性和催化应用
CuX 2（X = NO 3，Cl，Br，I）与四吡啶基官能化杯[4]芳烃在130°C的溶剂热反应制得四种新型配位聚合物，{[（（CuNO 3）2 L]·MeOH} n（1），[（CuCl 2）L 0.5 ] n（2），[（Cu 3 Br 3）L] n（3）和[（Cu 3 I 3）L] n（4），其中L = 25,26,27,28-四[（3-吡啶基甲基）氧基]杯[4]芳烃。所有产品均通过红外光谱，热重分析，单晶X射线衍射和粉末X射线衍射进行表征。晶体结构分析表明，1拥有由单核[Cu（NO 3）]单元和L个连接基构成的一维（1D）双链，而2个具有1D链，其碗形L配体起着连接连接基的作用。双核[Cu 2 Cl 4 ]单元。化合物3和4具有相似的二维网络，其中每个三核[Cu 3 Br 3 ] / [Cu 3 I3 ]单元充当三个连接节点，通过共享L个配体连接其六个等价物。这些结果表明，不同的阴离子对最终结构的形成具有重大影响。化合物1 - 4被用作催化剂为A 3微波辐射下偶联反应。值得注意的是，3显示出甲醛与各种炔烃和胺的A 3反应合成多功能炔丙胺的最佳催化性能（仅10分钟内收率高达94％）。
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