通过烷氧基配合物与酸反应合成含2,2':6',2"-三联吡啶的亚硝酰钌配合物。

Synthesis of nitrosylruthenium complexes containing 2,2':6',2"-terpyridine by reactions of alkoxo complexes with acids.

作者信息

Nagao Hirotaka, Enomoto Keiji, Wakabayashi Yuuki, Komiya Gen, Hirano Toshiyuki, Oi Takao

机构信息

Department of Chemistry, Faculty of Science and Technology, Sophia University, 7-1 Kioi-cho, Chiyoda-ku, Tokyo 102-8554, Japan.

出版信息

Inorg Chem. 2007 Feb 19;46(4):1431-9. doi: 10.1021/ic061644w.

DOI:10.1021/ic061644w

Abstract

Nitrosylruthenium complexes containing 2,2':6',2"-terpyridine (terpy) have been synthesized and characterized. The three alkoxo complexes trans-(NO, OCH3), cis-(Cl, OCH3)-[RuCl(OCH3)(NO)(terpy)]PF6 ([2]PF6), trans-(NO, OC2H5), cis-(Cl, OC2H5)-[RuCl(OC2H5)(NO)(terpy)]PF6 ([3]PF6), and [RuCl(OC3H7)(NO)(terpy)]PF6 ([4]PF6) were synthesized by reactions of trans-(Cl, Cl), cis-(NO, Cl)-[RuCl2(NO)(terpy)]PF6 ([1]PF6) with NaOCH3 in CH3OH, C2H5OH, and C3H7OH, respectively. Reactions of [3]PF6 with an acid such as hydrochloric acid and trifluoromethansulforic acid afford nitrosyl complexes in which the alkoxo ligand is substituted. The geometrical isomer of [1]PF6, trans-(NO, Cl), cis-(Cl, Cl)-[RuCl2(NO)(terpy)]PF6 ([5]PF6), was obtained by the reaction of [3]PF6 in a hydrochloric acid solution. Reaction of [3]PF6 with trifluoromethansulforic acid in CH3CN gave trans-(NO, Cl), cis-(CH3CN, Cl)-[RuCl(CH3CN)(NO)(terpy)]2+ ([6]2+) under refluxing conditions. The structures of [3]PF6, [4]PF6.CH3CN, [5]CF3SO3, and 62 were determined by X-ray crystallograpy.

摘要

已合成并表征了含2,2':6',2"-三联吡啶（terpy）的亚硝酰钌配合物。通过反式-(Cl, Cl)，顺式-(NO, Cl)-[RuCl2(NO)(terpy)]PF6（[1]PF6）分别与甲醇、乙醇和丙醇中的NaOCH3反应，合成了三种烷氧基配合物反式-(NO, OCH3)，顺式-(Cl, OCH3)-[RuCl(OCH3)(NO)(terpy)]PF6（[2]PF6）、反式-(NO, OC2H5)，顺式-(Cl, OC2H5)-[RuCl(OC2H5)(NO)(terpy)]PF6（[3]PF6）和[RuCl(OC3H7)(NO)(terpy)]PF6（[4]PF6）。[3]PF6与盐酸和三氟甲磺酸等酸反应，得到烷氧基配体被取代的亚硝酰配合物。通过[3]PF6在盐酸溶液中的反应，得到了[1]PF6的几何异构体反式-(NO, Cl)，顺式-(Cl, Cl)-[RuCl2(NO)(terpy)]PF6（[5]PF6）。在回流条件下，[3]PF6与三氟甲磺酸在乙腈中反应得到反式-(NO, Cl)，顺式-(CH3CN, Cl)-[RuCl(CH3CN)(NO)(terpy)]2+（[6]2+）。通过X射线晶体学确定了[3]PF6、[4]PF6·CH3CN、[5]CF3SO3和62的结构。

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