New Tetraruthenium Cluster from the Thermolysis of [Ru3(CO)10(μ-dppm)]: Crystal Structure of [HRu4(CO)9(μ3-PhPCH2PPh2) (μ3,η2:η1:η1-C6H4)]

IF 0.4 4区化学 Q4 CRYSTALLOGRAPHY Journal of Chemical Crystallography Pub Date : 2023-12-03 DOI:10.1007/s10870-023-00998-w

Md. Abdullah Al Mamun, Tazul Islam, Subas Rajbangshi, Shishir Ghosh, Michael G. Richmond, Shariff E. Kabir

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Abstract

Thermolysis of [Ru₃(CO)₁₀(μ-dppm)] (1) in refluxing benzene, followed by chromatographic separation by TLC, afforded the new cluster [HRu₄(CO)₉(μ₃-PhPCH₂PPh₂)(μ₃,η²:η¹:η¹-C₆H₄)] (10) in 7% yield in addition to the previously reported clusters [Ru₃(CO)₉{µ₃-PhPCH₂PPh(C₆H₄)}] (2) and [HRu₄(CO)₉(μ₄-PhPCH₂PPh₂)(μ₄,η⁶:η¹:η¹-C₆H₄)] (8) in 70% and 4% yields, respectively. The molecular structure of 10 has been determined by single-crystal X-ray diffraction analysis. Compound 10 possesses a Ru₄ metal core where two of the six triangular faces are capped by μ₃,η²:η¹:η¹-C₆H₄ (benzyne) and µ₃-PhPCH₂PPh₂ ligands. Compound 10 transforms to the known cluster [HRu₄(CO)₉(μ₃-PhPCH₂PPh₂)(μ₄,η⁶:η¹:η¹-C₆H₄)] (8) slowly at 80 °C. The bonding in the new cluster 10 has been investigated by electronic structure calculations.

Graphical Abstract

A new tetraruthenium cluster has been isolated and structurally characterized from the thermolysis of [Ru₃(CO)₁₀(μ-dppm)] at 80 °C.

Abstract Image

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[Ru3(CO)10(μ-dppm)]热裂解生成的新四钌团簇:[HRu4(CO)9(μ3- phpch2pph2) (μ3，η2:η1:η1- c6h4)]的晶体结构

[Ru3(CO)10(μ-dppm)](1)在回流苯中热分解，然后用薄层色谱分离，得到了新的团簇[HRu4(CO)9(μ3- phpch2pph2)(μ3，η2:η1 -C6H4)](10)，而先前报道的团簇[Ru3(CO)9{µ3-PhPCH2PPh(C6H4)}](2)和[HRu4(CO)9(μ4- phpch2pph2)(μ4，η6:η1 -C6H4)](8)的产率分别为70%和4%。通过单晶x射线衍射分析确定了10的分子结构。化合物10具有Ru4金属核，其中六个三角形面中有两个被μ3，η2:η1 - c6h4(苯基)和µ3-PhPCH2PPh2配体覆盖。化合物10在80℃时缓慢转变为已知簇[HRu4(CO)9(μ3-PhPCH2PPh2)(μ4，η6:η1 - c6h4)](8)。通过电子结构计算研究了新团簇10中的成键。从[Ru3(CO)10(μ-dppm)]在80℃下的热裂解反应中分离出了一个新的四砷团簇，并对其进行了结构表征。

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来源期刊

Journal of Chemical Crystallography 化学-光谱学

CiteScore

1.50

自引率

12.50%

发文量

审稿时长

6.3 months

期刊介绍： Journal of Chemical Crystallography is an international and interdisciplinary publication dedicated to the rapid dissemination of research results in the general areas of crystallography and spectroscopy. Timely research reports detail topics in crystal chemistry and physics and their relation to problems of molecular structure; structural studies of solids, liquids, gases, and solutions involving spectroscopic, spectrometric, X-ray, and electron and neutron diffraction; and theoretical studies.