State Key Lab for Physical Chemistry of Solid Surfaces, Department of Chemistry and College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, PR China.
Dalton Trans. 2011 Sep 7;40(33):8353-60. doi: 10.1039/c1dt10417a. Epub 2011 Jul 18.
This paper discusses the synthesis of two carbon-based pyridine ligands of fullerene pyrrolidine pyridine (C(60)-py) and multi-walled carbon nanotube pyrrolidine pyridine (MWCNT-py) via 1,3-dipolar cycloaddition. The two complexes, C(60)-Ru and MWCNT-Ru, were synthesized by ligand substitution in the presence of NH(4)PF(6), and Ru(II)(bpy)(2)Cl(2) was used as a reaction precursor. Both complexes were characterized by mass spectroscopy (MS), elemental analysis, nuclear magnetic resonance (NMR) spectroscopy, infrared spectroscopy (IR), ultraviolet/visible spectroscopy (UV-VIS) spectrometry, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and cyclic voltammetry (CV). The results showed that the substitution way of C(60)-py is different from that of MWCNT-py. The C(60)-py and a NH(3) replaced a Cl(-) and a bipyridine in Ru(II)(bpy)(2)Cl(2) to produce a five-coordinate complex of [Ru(bpy)(NH(3))(C(60)-py)Cl]PF(6), whereas MWCNT-py replaced a Cl(-) to generate a six-coordinate complex of [Ru(bpy)(2)(MWCNT-py)Cl]PF(6). The cyclic voltammetry study showed that the electron-withdrawing ability was different for C(60) and MWCNT. The C(60) showed a relatively stronger electron-withdrawing effect with respect to MWCNT.
本文讨论了通过 1,3-偶极环加成反应合成富勒烯吡咯吡啶(C(60)-py)和多壁碳纳米管吡咯吡啶(MWCNT-py)这两种基于碳的吡啶配体。在 NH(4)PF(6)存在下,通过配体取代反应合成了两种配合物 C(60)-Ru 和 MWCNT-Ru,反应前体为 Ru(II)(bpy)(2)Cl(2)。通过质谱(MS)、元素分析、核磁共振(NMR)光谱、红外光谱(IR)、紫外/可见光谱(UV-VIS)、拉曼光谱、X 射线光电子能谱(XPS)、热重分析(TGA)和循环伏安法(CV)对两种配合物进行了表征。结果表明,C(60)-py 的取代方式与 MWCNT-py 不同。C(60)-py 和一个 NH(3)取代了 Ru(II)(bpy)(2)Cl(2)中的一个 Cl(-)和一个联吡啶,生成了一个五配位的配合物[Ru(bpy)(NH(3))(C(60)-py)Cl]PF(6),而 MWCNT-py 取代了一个 Cl(-),生成了一个六配位的配合物[Ru(bpy)(2)(MWCNT-py)Cl]PF(6)。循环伏安法研究表明,C(60)和 MWCNT 的电子受主能力不同。C(60)相对于 MWCNT 具有更强的电子受主效应。