Chalcogen-centered spirocyclic mixed-metal carbonyl complexes: Synthesis and molecular structures of (CO)(8)(mu-PCy2)Re-2(mu(4)-E)Fe-2(mu-ER)(CO)(6) and [(CO)(8)(mu-PCy2)Re-2(mu(4)-E)Fe-2(CO)(6)](2)(mu(4)-E-2) (E = S, Se, Te; R organic residue)
DSpace at IIT Bombay
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Title |
Chalcogen-centered spirocyclic mixed-metal carbonyl complexes: Synthesis and molecular structures of (CO)(8)(mu-PCy2)Re-2(mu(4)-E)Fe-2(mu-ER)(CO)(6) and [(CO)(8)(mu-PCy2)Re-2(mu(4)-E)Fe-2(CO)(6)](2)(mu(4)-E-2) (E = S, Se, Te; R organic residue)
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Creator |
KLOSE, S
FLORKE, U EGOLD, H |
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Subject |
bridged dirhenium complexes
fe/e cluster complexes crystal-structures antimony-iron anions isomerization reactivity phosphorus ru3(co)12 so2cl2 |
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Description |
When NEt4[Re-2(mu-PCy2)(CO)(8)] (1) was reacted with Fe-2(mu-E-2)(CO)(6) (E = S, Se, TO in THF, the salts NEt4[(CO)(8)(mu-PCy2)Re-2(mu-E)Fe-2(mu-E)(CO)(6)] (E = S (2a), Se (2b), Te (2c)) were formed. Their spirocyclic anions were trapped with MeI, giving the spirocyclic complexes (CO)(8)(mu-PCy2)Re-2(mu(4)-E)Fe-2(mu-EMe)(CO)(6) (E = S (3a), Se (3b), Te (3c)). Their molecular structures were confirmed by single-crystal X-ray analysis. The anions of 2a-c are sensitive to oxidation. On crystallization in the presence of oxygen the corresponding dichalcogenides [(CO)(8)(mu-PCy2)Re-2(mu(4)-E)Fe-2(CO)(6)](2)(mu(4)-E-2) (E = S (4a), Se (4b), Te (4c)) were obtained in good yield. Their molecular structures were confirmed by single-crystal X-ray analysis. 2a was also trapped with CF3COOH, giving (CO)(8)(mu-PCy2)Re-2(mu-S-4)Fe-2(mu-SH)(CO)(6) (5). The latter can be expanded by SH oxidative addition of its mu-SH function to Os-3(CO)(11)(NCMe), giving the mixed-metal carbonyl complex (CO)(8)(mu-PCy2)Re-2(mu(4)-S)Fe-2(CO)(6)(mu(3)-S)Os-3(mu-H)(CO)(11) (6). The framework of 6 could be derived from X-ray diffraction data. However, these data were insufficient for complete solution of the molecular structure, but spectroscopic data and elemental analysis of 6 are in accordance with the proposed molecular structure.
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Publisher |
AMER CHEMICAL SOC
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Date |
2011-07-13T18:36:01Z
2011-12-26T12:48:02Z 2011-12-27T05:43:26Z 2011-07-13T18:36:01Z 2011-12-26T12:48:02Z 2011-12-27T05:43:26Z 2003 |
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Type |
Article
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Identifier |
ORGANOMETALLICS, 22(17), 3360-3366
0276-7333 http://dx.doi.org/10.1021/om030200u http://dspace.library.iitb.ac.in/xmlui/handle/10054/3743 http://hdl.handle.net/10054/3743 |
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Language |
en
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