轴向吡啶基配体羧酸铑(Ⅱ)的合成及表征  

Synthesis,Characterization of the Axial Pyridyl Ligand Rhodium(II)Carboxylate

作　　者：刘学 田乙然 童应成 倪文若 皮晓琳 李鸿鹏 袁藤瑞 张振强[1,2] Liu Xue;Tian Yiran;Tong Yingcheng;Ni Wenruo;Pi Xiaolin;Li Hongpeng;Yuan Tengrui;Zhang Zhenqiang(Kunming Institute of Precious Metals,Kunming 650106;Laboratory of Organic Complexes,Yunnan Precious Metals Laboratory Co.,Ltd.,Kunming 650106,China)

机构地区：[1]昆明贵金属研究所,云南昆明650106 [2]云南贵金属实验室有限公司有机配合物研究室,云南昆明650106

出　　处：《广东化工》2023年第13期11-15,共5页Guangdong Chemical Industry

基　　金：云南省基础研究专项-重点项目(202101AS070049);云南省贵金属新材料控股集团有限公司R&D项目(2020040602)。

摘　　要：本文由乙酸铑(Ⅱ)、三甲基乙酸铑(Ⅱ)与二溴-9-吡啶甲基-9H-咔唑配体(DBPMC)制备了4种羧酸铑(Ⅱ)轴向吡啶基配体羧酸铑配合物Rh_(2)(OOCR)4(DBPMC)_(2)。通过1H NMR、^(13)C NMR和FT-IR对这4种配合物进行表征,结果表明,这4种化合物属新型羧酸铑(Ⅱ)轴向配合物。成功培养得到Rh_(2)(OOCt-Bu)4(DBPMC3)_(2)化合物的单晶,通过X射线单晶衍射分析确定,配体分子中吡啶-4-基的氮原子和三甲基乙酸铑(Ⅱ)轴向进行配位,每个铑原子都处于轻微扭曲的八面体环境中心,并绘制了其分子结构图及晶胞堆积图。Four rhodium(II)carboxylate axial pyridyl ligands Rh_(2)(OOCR)4(DBPMC)_(2) were prepared by rhodium(II)acetate,rhodium(II)trimethylacetate and dibromo-9-pyridylmethyl-9H-carbazole ligand(DBPMC),respectively.These 4 compounds characterized by 1H NMR,^(13)C NMR and IR,and the results showed that these four compounds were novel rhodium(II)carboxylate axial complexes.At the same time,single crystals of Rh_(2)(OOCt-Bu)4(DBPMC3)_(2) were successfully grown,and characterized by single-crystal X-ray.The structure of compounds showed that the nitrogen atom of pyridin-4-based and rhodium(II)trimethylacetate were coordinated axially in the ligand molecule,and each rhodium atom was at the center of the slightly distorted octahedral environment,and its molecular structure and unit cell stacking map were drawn.

关 键 词：乙酸铑(Ⅱ) 三甲基乙酸铑(Ⅱ) 轴向配位 晶体结构 合成 

分 类 号：TQ[化学工程]