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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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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)
 
Creator KLOSE, S
FLORKE, U
EGOLD, H
 
Subject bridged dirhenium complexes
fe/e cluster complexes
crystal-structures
antimony-iron
anions
isomerization
reactivity
phosphorus
ru3(co)12
so2cl2
 
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.
 
Publisher AMER CHEMICAL SOC
 
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
 
Type Article
 
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
 
Language en