新型铑(Ⅱ)配合物的合成及晶体结构

doi:10.13438/j.cnki.jdzk.2023.04.007

吉首大学学报（自然科学版） ›› 2023, Vol. 44 ›› Issue (4): 55-68.DOI: 10.13438/j.cnki.jdzk.2023.04.007

新型铑(Ⅱ)配合物的合成及晶体结构

刘学,田乙然，冯洋洋，许明明，陈洪来，侯文明，张振强，刘伟平

(1.贵研铂业股份有限公司，云南昆明 650106；2.云南贵金属实验室有限公司，云南昆明 650106；3.昆明贵金属研究所稀贵金属综合利用新技术国家重点实验室，云南昆明 650106）

出版日期:2023-07-25 发布日期:2023-07-26
通讯作者: 侯文明（1978—），男，山西临汾人，贵研铂业股份有限公司化学高级工程师，主要从事贵金属化学研究.E-mail:hwm@ipm.com.cn.
作者简介:刘学（1992—），男，江苏徐州人，硕士，主要从事铂族金属均相催化剂研究；田乙然（1997—），女，云南昆明人，硕士，主要从事贵金属无机精细化学品研究，与刘学为共同第一作者
基金资助:
云南省基础研究专项-重点项目（0101AS070049）；云南省贵金属新材料控股集团有限公司R&D项目（0004060）

Synthesis,Crystal Structure of the Novel Rhodium（Ⅱ） Complex

LIU Xue,TIAN Yiran,FENG Yangyang,XU Mingming,CHEN Honglai,HOU Wenming,ZHANG Zhenqiang,LIU Weiping

(1.State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals,Kunming 650106,Yunnan China;.Yunnan Precious Metals Laboratory Co.,Ltd.,Kunming 650106,Yunnan China;3.Sino-Platinum Metals Co.Ltd.,Kunming 650106,Yunnan China)

Online:2023-07-25 Published:2023-07-26

摘要/Abstract

摘要：选择乙酸铑（Ⅱ）、三甲基乙酸铑（Ⅱ）为主体，以3,6-二溴-9-(4-吡啶甲基)-9H-咔唑（DBPMC1）、3,6-二溴-9-(3-吡啶甲基)-9H-咔唑（DBPMC2）为轴向配体，设计并合成了4种羧酸铑（Ⅱ）轴向二溴-9-吡啶甲基-9H-咔唑配合物Rh₂(OOCR)₄(DBPMC)₂，并成功培养其单晶；采用现代分析手段，如核磁共振H谱（H NMR）、核磁共振C谱（¹³C NMR）和傅里叶变换红外光谱（FT-IR）等初步表征了4种配合物的化学结构.结果表明，这4种化合物均未见有文献报道，属新型羧酸铑（Ⅱ）轴向配合物.通过X射线单晶衍射分析确定，配合物是由一分子的羧酸铑（Ⅱ）和两分子的DBPMC配体配位而成，所得结构符合预期实验设计.

关键词： 羧酸铑（Ⅱ）, 轴向配位, 晶体结构, 分子结构图, 晶胞堆积图

Abstract: Using rhodium（Ⅱ） acetate and trimethylrhodium acetate（Ⅱ） as the raw material,with 3,6-dibromo-9-(4-pyridinemethyl)-9H-carbazole (DBPMC1) and 3,6-dibromo-9-(3-pyridinemethyl)-9H-carbazole (DBPMC) as axial ligands,four rhodium（Ⅱ） carboxylates axial dibromo-9-pyridylmethyl-9H-carbazole complexes Rh(OOCR)4(DBPMC) were designed and synthesized.The single crystals of compounds were successfully cultured and their chemical structures were initially characterized by modern analytical methods such as H NMR,13C NMR and FT-IR.The results show that none of these four compounds has been reported in the literature,and they belong to a new type of rhodium carboxylate （Ⅱ） axial complex.The structure of the complex was determined by X-ray single crystal diffraction analysis to be composed of one molecule of rhodium（Ⅱ） carboxylate and two molecules of DBPMC ligand,and the molecular structure diagram and unit cell stacking diagram were drawn.

Key words: rhodium（Ⅱ） acetate, axial coordination, crystal structure, molecular structure diagram, cell stacking diagram

刘学, 田乙然, 冯洋洋, 许明明, 陈洪来, 侯文明, 张振强, 刘伟平. 新型铑(Ⅱ)配合物的合成及晶体结构[J]. 吉首大学学报（自然科学版）, 2023, 44(4): 55-68.

LIU Xue, TIAN Yiran, FENG Yangyang, XU Mingming, CHEN Honglai, HOU Wenming, ZHANG Zhenqiang, LIU Weiping. Synthesis,Crystal Structure of the Novel Rhodium（Ⅱ） Complex[J]. Journal of Jishou University(Natural Sciences Edition), 2023, 44(4): 55-68.

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新型铑(Ⅱ)配合物的合成及晶体结构

Synthesis,Crystal Structure of the Novel Rhodium（Ⅱ） Complex

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