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Synthesis and structure of metallacarboranes bearing carborane-fused cyclopentenyl and dicarbollyl-fused cyclopentene ligands
Dalton Transactions ( IF 3.5 ) Pub Date : 2021-06-29 , DOI: 10.1039/d1dt01592c Tek Long Chan 1 , Zhenpin Lu 1 , Zuowei Xie 1
Dalton Transactions ( IF 3.5 ) Pub Date : 2021-06-29 , DOI: 10.1039/d1dt01592c Tek Long Chan 1 , Zhenpin Lu 1 , Zuowei Xie 1
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New types of ligands, carborane-fused cyclopentenyl and dicarbollyl-fused cyclopentene, were conveniently prepared in high yields. Treatment of the lithium salt of carborane-fused cyclopentenyl anion, [1,2-[C(Me)CHC(Ph)]-1,2-C2B10H10]Li, with [Cp*RuCl]4 generated an 18-electron complex [η3:η2-(PhCCHCMe)C2B10H10]Ru(η5-Cp*). On the other hand, reaction of the dicarbollide salt, [7,8-(CH2CH![[double bond, length as m-dash]](https://www.rsc.org/images/entities/char_e001.gif)
CMe)-7,8-C2B9H9]Na2 with [(η6-p-cymene)RuCl2]2 or CoCl2/CpNa, afforded the salt metathesis product [η5-(CH2CHCMe)C2B9H9]Ru(η6-p-cymene) or [η5-(CH2CHCMe)C2B9H9]Co(η5-C5H5) in good yields. In contrast, [7,8-(CH2CHCMe)-7,8-C2B9H9]Na2 reacted with Ni(dppp)Cl2 (dppp = 1,3-bis(diphenylphosphino)propane) to give another 18-electron metallacarborane [η5-(CH2CHCMe)C2B9H9]Ni(dppp), in which one of the cage carbon atoms has been isomerized to the lower belt of the cage due to steric reasons. All these new metallacarborane compounds were fully characterized by NMR spectroscopy, high-resolution mass spectroscopy and single-crystal X-ray analyses.
中文翻译：
含碳硼烷稠合环戊烯基和二羰基稠合环戊烯配体的金属碳硼烷的合成与结构
新型配体，碳硼烷稠合的环戊烯基和二羰基稠合的环戊烯，可以以高产率方便地制备。用 [Cp*RuCl] 4处理碳硼烷稠合的环戊烯基阴离子的锂盐 [1,2-[C(Me)CHC(Ph)]-1,2-C 2 B 10 H 10 ]Li，生成18-电子络合物[η 3 :η 2 -(PhCCHCMe)C 2 B 10 H 10 ]Ru(η 5 -Cp*)。另一方面，二碳化物盐，[7,8-(CH 2 CH CMe)-7,8-C 2 B 9 H 9 ]Na 2与 [(η 6- p -伞花烃)RuCl 2 ] 2或CoCl 2 /CpNa，得到盐复分解产物[η 5 -(CH 2 CH CMe)C 2 B 9 H 9 ]Ru(η 6 - p -伞花烃)或[η 5 -(CH 2 CH CMe)C 2 B 9 H 9 ]Co(η 5 -C 5 H 5 ) 收率良好。相反，[7,8-(CH 2 CH CMe)-7,8-C 2 B 9 H 9 ]Na2与 Ni(dppp)Cl 2 (dppp = 1,3-双(二苯基膦)丙烷)反应得到另一个 18-电子金属碳硼烷 [η 5 -(CH 2 CHCMe)C 2 B 9 H 9 ]Ni(dppp) ，其中一个笼碳原子由于空间原因已异构化到笼的下部带。所有这些新的金属碳硼烷化合物都通过核磁共振光谱、高分辨率质谱和单晶 X 射线分析进行了充分表征。
更新日期：2021-07-21
CMe)-7,8-C2B9H9]Na2 with [(η6-p-cymene)RuCl2]2 or CoCl2/CpNa, afforded the salt metathesis product [η5-(CH2CHCMe)C2B9H9]Ru(η6-p-cymene) or [η5-(CH2CHCMe)C2B9H9]Co(η5-C5H5) in good yields. In contrast, [7,8-(CH2CHCMe)-7,8-C2B9H9]Na2 reacted with Ni(dppp)Cl2 (dppp = 1,3-bis(diphenylphosphino)propane) to give another 18-electron metallacarborane [η5-(CH2CHCMe)C2B9H9]Ni(dppp), in which one of the cage carbon atoms has been isomerized to the lower belt of the cage due to steric reasons. All these new metallacarborane compounds were fully characterized by NMR spectroscopy, high-resolution mass spectroscopy and single-crystal X-ray analyses.
中文翻译：
含碳硼烷稠合环戊烯基和二羰基稠合环戊烯配体的金属碳硼烷的合成与结构
新型配体，碳硼烷稠合的环戊烯基和二羰基稠合的环戊烯，可以以高产率方便地制备。用 [Cp*RuCl] 4处理碳硼烷稠合的环戊烯基阴离子的锂盐 [1,2-[C(Me)CHC(Ph)]-1,2-C 2 B 10 H 10 ]Li，生成18-电子络合物[η 3 :η 2 -(PhCCHCMe)C 2 B 10 H 10 ]Ru(η 5 -Cp*)。另一方面，二碳化物盐，[7,8-(CH 2 CH CMe)-7,8-C 2 B 9 H 9 ]Na 2与 [(η 6
- p -伞花烃)RuCl 2 ] 2或CoCl 2 /CpNa，得到盐复分解产物[η 5 -(CH 2 CH CMe)C 2 B 9 H 9 ]Ru(η 6 - p -伞花烃)或[η 5 -(CH 2 CH CMe)C 2 B 9 H 9 ]Co(η 5 -C 5 H 5 ) 收率良好。相反，[7,8-(CH 2 CH CMe)-7,8-C 2 B 9 H 9 ]Na2与 Ni(dppp)Cl 2 (dppp = 1,3-双(二苯基膦)丙烷)反应得到另一个 18-电子金属碳硼烷 [η 5 -(CH 2 CHCMe)C 2 B 9 H 9 ]Ni(dppp) ，其中一个笼碳原子由于空间原因已异构化到笼的下部带。所有这些新的金属碳硼烷化合物都通过核磁共振光谱、高分辨率质谱和单晶 X 射线分析进行了充分表征。
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