Köhn Randolf D, Tomás Laudo Lorena, Pan Zhida, Speiser Fredy, Kociok-Köhn Gabriele
Department of Chemistry, University of Bath, Bath, UKBA2 7AY.
Dalton Trans. 2009 Jun 21(23):4556-68. doi: 10.1039/b819268e. Epub 2009 Apr 2.
Triazacyclohexanes (R(3)TAC,1a-i ) with pyridyl or thioether functionalities (R) in the N-substituents react with three equivalents of CuX (X = Cl (2), Br (3) or I (4)) in MeCN to give the triangular tri-copper clusters [R(3)TAC(CuX)(3)] (R = 2-pyridylmethyl (2a, 3a ), 5-(t)butyl-2-pyridyl (3b). 2-(3-phenylpropylthio)ethyl (3c), 2-(2-ethyl-butylthio)ethyl (3d), 2-(4-heptylthio)ethyl (2e, 3e ), 2-(1-heptylthio)ethyl (3f), 2-(2,4,6-trimethyl-benzylthio)ethyl (3g), 2-(o-methyl-benzylthio)ethyl (3h) and 2-(o-fluoro-benzylthio)ethyl (2i, 3i 4i)). The thioether complexes are stable towards air and water. The bromide bridge in the clusters can be replaced by chloride (2c, e, f, i) or iodide (4c, e, f, i ) by the reaction of a dichloromethane solution of the cluster with aqueous NaI or AgCl, respectively. Crystal structures of 2a, 3a, 3b, 2e, 3h and show triangular halide-bridged Cu(3) clusters capped by the triazacyclohexane and stabilised by the coordination of one pyridyl or thioether arm to each copper atom. DFT calculations confirm the NMR assignments and reveal the electronic structure of the copper triangle.
在N-取代基中带有吡啶基或硫醚官能团(R)的三氮杂环己烷(R(3)TAC,1a-i)与三当量的CuX(X = Cl(2)、Br(3)或I(4))在乙腈中反应,生成三角形三铜簇[R(3)TAC(CuX)(3)](R = 2-吡啶基甲基(2a,3a)、5-叔丁基-2-吡啶基(3b)、2-(3-苯丙基硫基)乙基(3c)、2-(2-乙基丁基硫基)乙基(3d)、2-(4-庚基硫基)乙基(2e,3e)、2-(1-庚基硫基)乙基(3f)、2-(2,4,6-三甲基苄基硫基)乙基(3g)、2-(邻甲基苄基硫基)乙基(3h)和2-(邻氟苄基硫基)乙基(2i,3i,4i))。硫醚配合物对空气和水稳定。通过使簇的二氯甲烷溶液分别与NaI水溶液或AgCl反应,簇中的溴桥可以被氯(2c、e、f、i)或碘(4c、e、f、i)取代。2a、3a、3b、2e、3h的晶体结构显示,三角形卤化物桥连的Cu(3)簇由三氮杂环己烷封端,并通过每个铜原子与一个吡啶基或硫醚臂的配位作用而稳定。密度泛函理论计算证实了核磁共振归属,并揭示了铜三角形的电子结构。