Klose, Stefanie ; Florke, Ulrich ; Egold, Hans ; Mathur, Pradeep (2003) Chalcogen-centered spirocyclic mixed-metal carbonyl complexes: Synthesis and molecular structures of (CO)8(μ-PCy2)Re2(μ4-E)Fe2(μ-ER)(CO)6 and [(CO)8(μ-PCy2)Re2(μ4-E)Fe2(CO)6]2(μ4-E2) (E = S, Se, Te; R = Organic Residue) Organometallics, 22 (17). pp. 3360-3366. ISSN 0276-7333
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Official URL: http://pubs.acs.org/doi/abs/10.1021/om030200u
Related URL: http://dx.doi.org/10.1021/om030200u
Abstract
When NEt4[Re2(μ-PCy2)(CO)8] (1) was reacted with Fe2(μ-E2)(CO)6 (E = S, Se, Te) in THF, the salts NEt4[(CO)8(μ-PCy2)Re2(μ4-E)Fe2(μ-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(μ-PCy2)Re2(μ4-E)Fe2(μ-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(μ-PCy2)Re2(μ4-E)Fe2(CO)6]2(μ4-E2) (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(μ-PCy2)Re2(μ-S4)Fe2(μ-SH)(CO)6 (5). The latter can be expanded by SH oxidative addition of its μ-SH function to Os3(CO)11(NCMe), giving the mixed-metal carbonyl complex (CO)8(μ-PCy2)Re2(μ4-S)Fe2(CO)6(μ3-S)Os3(μ-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.
| Item Type: | Article |
|---|---|
| Source: | Copyright of this article belongs to American Chemical Society. |
| ID Code: | 24870 |
| Deposited On: | 01 Dec 2010 12:37 |
| Last Modified: | 01 Mar 2011 05:03 |
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