A Bis(silylenyl)pyridine Zero-Valent Germanium Complex and Its Remarkable Reactivity
The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0→Fe(CO)4 is reported. The compound was obtained in 49 % yield from the reaction of the bis(N‐heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6‐C5NH3‐[EtNSi(NtBu)2CPh]2) with GeCl2⋅(diox...
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| Published in | Angewandte Chemie International Edition Vol. 55; no. 48; pp. 15096 - 15099 |
|---|---|
| Main Authors | , , , , |
| Format | Journal Article |
| Language | English |
| Published |
Germany
Blackwell Publishing Ltd
21.11.2016
Wiley Subscription Services, Inc |
| Edition | International ed. in English |
| Subjects | |
| Online Access | Get full text |
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| Abstract | The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0→Fe(CO)4 is reported. The compound was obtained in 49 % yield from the reaction of the bis(N‐heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6‐C5NH3‐[EtNSi(NtBu)2CPh]2) with GeCl2⋅(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]GeIICl+ Cl−, which was further reduced with K2Fe(CO)4. Single‐crystal X‐ray diffraction analysis of [SiNSi]Ge→Fe(CO)4 revealed that the Ge0 center adopts a trigonal‐pyramidal geometry with a Si‐Ge‐Si angle of 95.66(2)°. Remarkably, one of the SiII donor atoms in the complex is five‐coordinated because of additional (pyridine)N→Si coordination. Unexpectedly, the reaction of [SiNSi]Ge→Fe(CO)4 with GeCl2⋅(dioxane) (one molar equivalent) yielded the first push–pull germylone–germylene donor–acceptor complex, [SiNSi]Ge→GeCl2→Fe(CO)4 through the insertion of GeCl2 into the dative Ge0→Fe bond. The electronic features of the new compounds were investigated by DFT calculations.
Germanium‐enriched: The synthesis and unusual chemical and electronic properties of the first zero‐valent germanium (“germylone”) iron complex [SiNSi]GeFe(CO)4 are reported. This complex was further transformed into an unprecedented mixed‐valent push–pull Ge0→GeCl2 complex. |
|---|---|
| AbstractList | The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge
→Fe(CO)
is reported. The compound was obtained in 49 % yield from the reaction of the bis(N-heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6-C
NH
-[EtNSi(N
Bu)
CPh]
) with GeCl
⋅(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]Ge
Cl
Cl
, which was further reduced with K
Fe(CO)
. Single-crystal X-ray diffraction analysis of [SiNSi]Ge→Fe(CO)
revealed that the Ge
center adopts a trigonal-pyramidal geometry with a Si-Ge-Si angle of 95.66(2)°. Remarkably, one of the Si
donor atoms in the complex is five-coordinated because of additional (pyridine)N→Si coordination. Unexpectedly, the reaction of [SiNSi]Ge→Fe(CO)
with GeCl
⋅(dioxane) (one molar equivalent) yielded the first push-pull germylone-germylene donor-acceptor complex, [SiNSi]Ge→GeCl
→Fe(CO)
through the insertion of GeCl
into the dative Ge
→Fe bond. The electronic features of the new compounds were investigated by DFT calculations. The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge 0 →Fe(CO) 4 is reported. The compound was obtained in 49 % yield from the reaction of the bis(N‐heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6‐C 5 NH 3 ‐[EtNSi(N t Bu) 2 CPh] 2 ) with GeCl 2 ⋅(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]Ge II Cl + Cl − , which was further reduced with K 2 Fe(CO) 4 . Single‐crystal X‐ray diffraction analysis of [SiNSi]Ge →Fe(CO) 4 revealed that the Ge 0 center adopts a trigonal‐pyramidal geometry with a Si‐Ge‐Si angle of 95.66(2)°. Remarkably, one of the Si II donor atoms in the complex is five‐coordinated because of additional (pyridine)N→Si coordination. Unexpectedly, the reaction of [SiNSi]Ge →Fe(CO) 4 with GeCl 2 ⋅(dioxane) (one molar equivalent) yielded the first push–pull germylone–germylene donor–acceptor complex, [SiNSi]Ge →GeCl 2 →Fe(CO) 4 through the insertion of GeCl 2 into the dative Ge 0 →Fe bond. The electronic features of the new compounds were investigated by DFT calculations. The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0 →Fe(CO)4 is reported. The compound was obtained in 49 % yield from the reaction of the bis(N-heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6-C5 NH3 -[EtNSi(Nt Bu)2 CPh]2 ) with GeCl2 ⋅(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]GeII Cl+ Cl- , which was further reduced with K2 Fe(CO)4 . Single-crystal X-ray diffraction analysis of [SiNSi]Ge→Fe(CO)4 revealed that the Ge0 center adopts a trigonal-pyramidal geometry with a Si-Ge-Si angle of 95.66(2)°. Remarkably, one of the SiII donor atoms in the complex is five-coordinated because of additional (pyridine)N→Si coordination. Unexpectedly, the reaction of [SiNSi]Ge→Fe(CO)4 with GeCl2 ⋅(dioxane) (one molar equivalent) yielded the first push-pull germylone-germylene donor-acceptor complex, [SiNSi]Ge→GeCl2 →Fe(CO)4 through the insertion of GeCl2 into the dative Ge0 →Fe bond. The electronic features of the new compounds were investigated by DFT calculations.The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0 →Fe(CO)4 is reported. The compound was obtained in 49 % yield from the reaction of the bis(N-heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6-C5 NH3 -[EtNSi(Nt Bu)2 CPh]2 ) with GeCl2 ⋅(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]GeII Cl+ Cl- , which was further reduced with K2 Fe(CO)4 . Single-crystal X-ray diffraction analysis of [SiNSi]Ge→Fe(CO)4 revealed that the Ge0 center adopts a trigonal-pyramidal geometry with a Si-Ge-Si angle of 95.66(2)°. Remarkably, one of the SiII donor atoms in the complex is five-coordinated because of additional (pyridine)N→Si coordination. Unexpectedly, the reaction of [SiNSi]Ge→Fe(CO)4 with GeCl2 ⋅(dioxane) (one molar equivalent) yielded the first push-pull germylone-germylene donor-acceptor complex, [SiNSi]Ge→GeCl2 →Fe(CO)4 through the insertion of GeCl2 into the dative Ge0 →Fe bond. The electronic features of the new compounds were investigated by DFT calculations. The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0→Fe(CO)4 is reported. The compound was obtained in 49 % yield from the reaction of the bis(N‐heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6‐C5NH3‐[EtNSi(NtBu)2CPh]2) with GeCl2⋅(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]GeIICl+ Cl−, which was further reduced with K2Fe(CO)4. Single‐crystal X‐ray diffraction analysis of [SiNSi]Ge→Fe(CO)4 revealed that the Ge0 center adopts a trigonal‐pyramidal geometry with a Si‐Ge‐Si angle of 95.66(2)°. Remarkably, one of the SiII donor atoms in the complex is five‐coordinated because of additional (pyridine)N→Si coordination. Unexpectedly, the reaction of [SiNSi]Ge→Fe(CO)4 with GeCl2⋅(dioxane) (one molar equivalent) yielded the first push–pull germylone–germylene donor–acceptor complex, [SiNSi]Ge→GeCl2→Fe(CO)4 through the insertion of GeCl2 into the dative Ge0→Fe bond. The electronic features of the new compounds were investigated by DFT calculations. Germanium‐enriched: The synthesis and unusual chemical and electronic properties of the first zero‐valent germanium (“germylone”) iron complex [SiNSi]GeFe(CO)4 are reported. This complex was further transformed into an unprecedented mixed‐valent push–pull Ge0→GeCl2 complex. The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0[arrow right]Fe(CO)4 is reported. The compound was obtained in 49% yield from the reaction of the bis(N-heterocyclic silylenyl)pyridine pincer ligand SiNSi (1,6-C5NH3-[EtNSi(NtBu)2CPh]2) with GeCl2(dioxane) to give the corresponding chlorogermyliumylidene chloride precursor [SiNSi]GeIICl+Cl-, which was further reduced with K2Fe(CO)4. Single-crystal X-ray diffraction analysis of [SiNSi]Ge[arrow right]Fe(CO)4 revealed that the Ge0 center adopts a trigonal-pyramidal geometry with a Si-Ge-Si angle of 95.66(2)°. Remarkably, one of the SiII donor atoms in the complex is five-coordinated because of additional (pyridine)N[arrow right]Si coordination. Unexpectedly, the reaction of [SiNSi]Ge[arrow right]Fe(CO)4 with GeCl2(dioxane) (one molar equivalent) yielded the first push-pull germylone-germylene donor-acceptor complex, [SiNSi]Ge[arrow right]GeCl2[arrow right]Fe(CO)4 through the insertion of GeCl2 into the dative Ge0[arrow right]Fe bond. The electronic features of the new compounds were investigated by DFT calculations. |
| Author | Zhou, Yu-Peng Apeloig, Yitzhak Yao, Shenglai Driess, Matthias Karni, Miriam |
| Author_xml | – sequence: 1 givenname: Yu-Peng surname: Zhou fullname: Zhou, Yu-Peng organization: Department of Chemistry, Metalorganics and Inorganic Materials, Sekr. C2, Technische Universität Berlin, Strasse des 17. Juni 135, 10623, Berlin, Germany – sequence: 2 givenname: Miriam surname: Karni fullname: Karni, Miriam organization: Schulich Department of Chemistry and the Lise Meitner Minerva Center for Computational Chemistry, Technion, Israel Institute of Technology, 32000, Haifa, Israel – sequence: 3 givenname: Shenglai surname: Yao fullname: Yao, Shenglai organization: Department of Chemistry, Metalorganics and Inorganic Materials, Sekr. C2, Technische Universität Berlin, Strasse des 17. Juni 135, 10623, Berlin, Germany – sequence: 4 givenname: Yitzhak surname: Apeloig fullname: Apeloig, Yitzhak email: apeloig@technion.ac.il organization: Schulich Department of Chemistry and the Lise Meitner Minerva Center for Computational Chemistry, Technion, Israel Institute of Technology, 32000, Haifa, Israel – sequence: 5 givenname: Matthias surname: Driess fullname: Driess, Matthias email: matthias.driess@tu-berlin.de organization: Department of Chemistry, Metalorganics and Inorganic Materials, Sekr. C2, Technische Universität Berlin, Strasse des 17. Juni 135, 10623, Berlin, Germany |
| BackLink | https://www.ncbi.nlm.nih.gov/pubmed/27804223$$D View this record in MEDLINE/PubMed |
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| Copyright | 2016 Wiley‐VCH Verlag GmbH & Co. KGaA, Weinheim 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim. 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim |
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| Keywords | metallylenes pincer ligands silicon germanium silylene |
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| Snippet | The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0→Fe(CO)4 is reported. The compound was obtained in... The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge 0 →Fe(CO) 4 is reported. The compound was obtained... The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge →Fe(CO) is reported. The compound was obtained in... The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0[arrow right]Fe(CO)4 is reported. The compound was... The synthesis, reactivity, and electronic structure of the unique germylone iron carbonyl complex [SiNSi]Ge0 →Fe(CO)4 is reported. The compound was obtained in... |
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| SubjectTerms | Carbonyl compounds Germanium metallylenes pincer ligands silicon silylene X-ray diffraction |
| Title | A Bis(silylenyl)pyridine Zero-Valent Germanium Complex and Its Remarkable Reactivity |
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