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| 两种乙酰丙酮.羰基铑化合物的合成与晶体结构表征 |
| Synthesis and Crystal Structure Characterization of Two Rhodium Carbonyl Compounds |
| Received:October 20, 2015 |
| DOI： |
| 中文关键词: 有机化学 乙酰丙酮.二羰基铑 乙酰丙酮.三苯基膦.羰基铑 合成 晶体结构 |
| 英文关键词: organic chemistry [Rh(CO)2(acac)]2 Rh(acac)(PPh3)(CO) synthesis crystal structure |
| 基金项目:国家科技支撑计划(2012BAE06B08)、云南省科技创新(2015AA006)、稀贵金属国家重点实验室开放课题(2014020605) |
| Author Name | Affiliation | E-mail | | YU Juan | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | juanyu1210@126.com | | YE Qingsong | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | | | SHEN Shanwen | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | shensw@ipm.com.cn | | ZUO Chuan | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | | | LIU Guihua | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | | | LIU Weiping | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | |
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| 中文摘要: |
| 在N,N-二甲基甲酰胺介质中，将水合三氯化铑与乙酰丙酮加热回流，一步合成了乙酰丙酮.二羰基铑([Rh(CO)2(acac)]2)，产率为93%；以正丁烷为介质，[Rh(CO)2(acac)]2与三苯基磷(PPh3)定量反应，得到乙酰丙酮.三苯基膦.羰基铑(Rh(acac)(PPh3)(CO))，产率为99%。用气相扩散法和溶剂缓慢挥发法分别培养出[Rh(CO)2(acac)]2和Rh(acac)(PPh3)(CO)单晶，元素分析的结果表明产物为目标化合物。用X射线单晶衍射仪对其结构进行了表征，获得了晶体结构参数，结果表明2种化合物均为三斜晶系、P-1空间群，[Rh(CO)2(acac)]2为二聚体化合物，Rh(acac)(PPh3)(CO)为单核配合物。 |
| 英文摘要: |
| [Rh(CO)2(acac)]2 was synthesized in one-step process from RhCl3.3H2O in DMF by adding acac as the anion ligand. The yield was 93%. A quantitative reaction between [Rh(CO)2(acac)]2 and PPh3 in n-butane gave rise to the formation of Rh(acac)(PPh3)(CO) with a yield of 99%. Single crystals of two complexes were prepared, respectively, via a gaseous diffusion method and a solvent evaporation technique, and were subjected to X-ray diffraction analysis. The results show both complexes are in the triclinic system with a space group of P-1. [Rh(CO)2(acac)]2 displays a dimmeric structure with Rh-Rh bond being 3.417 ?, whereas Rh(acac)(PPh3)(CO) has a normal mononuclear structure. |
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