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首页> 外文期刊>RSC Advances >Palladium(II) complexes bearing the 1,2,3-triazole based organosulfur/selenium ligand: synthesis, structure and applications in Heck and Suzuki-Miyaura coupling as a catalyst via palladium nanoparticles
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Palladium(II) complexes bearing the 1,2,3-triazole based organosulfur/selenium ligand: synthesis, structure and applications in Heck and Suzuki-Miyaura coupling as a catalyst via palladium nanoparticles

机译：带有1,2,3-三唑基有机硫/硒配体的钯（II）配合物：通过钯纳米粒子作为催化剂在Heck和Suzuki-Miyaura偶联中的合成，结构和应用

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摘要

Air and moisture insensitive palladium complexes, [Pd(L)Cl-2] (1/2), in which L = 1-benzyl-4-phenylthiomethyl or 1-benzyl-4-phenylselenomethyl-1H-1,2,3-triazole (L1 or L2) catalyze Heck (HC) and Suzuki-Miyaura coupling (SMC) reactions between a series of aryl bromides including deactivated bromides and n-butyl acrylate and phenylboronic acid, respectively. The optimal catalytic loading was found to be in the order of 0.01 mol%. HRTEM, TGA and EDX data indicated that 3-11 nm nanoparticles (NPs) composed of palladium and sulfur or selenium and protected with L or its fragment, were formed during the catalyzed reaction. The isolated NPs displayed catalytic activity and appeared to have a role in the catalysis. A two-phase test indicated that both homogeneous and heterogeneous catalysis took place. The complexes 1 and 2 were synthesized by the reactions of L1 and L2 respectively with [(MeCN)(2)PdCl2]. Their single crystal X-ray diffraction indicated that the geometry adopted by ligands around Pd in both complexes is distorted square planar with Pd-S and Pd-Se bond lengths of 2.2727(14) and 2.3693(8) angstrom, respectively. DFT calculation gave bond lengths and angles in keeping with the experimental values. The DFT calculated HOMO-LUMO energy difference is lower for 1 than for 2 in accordance with the observed higher catalytic activity of 1.
机译：对空气和湿气不敏感的钯配合物[Pd（L）Cl-2]（1/2），其中L = 1-苄基-4-苯基硫甲基或1-苄基-4-苯基硒甲基-1H-1,2,3-三唑（L1或L2）分别催化一系列芳基溴化物（包括失活的溴化物和丙烯酸正丁酯和苯基硼酸）之间的Heck（HC）和Suzuki-Miyaura偶联（SMC）反应。发现最佳的催化负载量约为0.01mol％。 HRTEM，TGA和EDX数据表明，在催化反应过程中形成了由钯和硫或硒组成并受L或其片段保护的3-11 nm纳米颗粒（NPs）。分离出的NP显示出催化活性并且似乎在催化中起作用。两阶段试验表明均相和异相催化均发生。通过L1和L2分别与[（MeCN）（2）PdCl2]反应合成配合物1和2。他们的单晶X射线衍射表明，两种配合物中Pd周围的配体所采用的几何形状都是扭曲的正方形平面，Pd-S和Pd-Se的键长分别为2.2727（14）和2.3693（8）埃。 DFT计算得出键合长度和角度与实验值一致。 DFT计算得出的HOMO-LUMO能量差比1的2低，这是因为观察到的1的较高催化活性。

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