Hexamethyl-1,2,3-tristanna-[3]ferrocenophane – Molecular Structure and Cleavage of the Tin–Tin Bonds by Iodine, Sulfur, Selenium, and Tellurium
✍ Scribed by Max Herberhold; Udo Steffl; Wolfgang Milius; Bernd Wrackmeyer
- Publisher
- John Wiley and Sons
- Year
- 1998
- Tongue
- German
- Weight
- 189 KB
- Volume
- 624
- Category
- Article
- ISSN
- 0372-7874
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✦ Synopsis
2,
ferrocenophane (1) was prepared by the reaction of 1,1'-bis(dimethylstannyl)ferrocene (3) with bis(diethylamino)dimethylstannane. The molecular structure of 1 was determined by X-ray crystallography. The monoclinic unit cell (space group P2 1 /c; a = 18.659(4), b = 17.311(3), c = 13.719(3) A Ê ; b = 111.02(3)°) contains two independent molecules which differ slightly in their conformation. The cyclopentadienyl rings are almost parallel, but the positions of the substituted carbon atoms are twisted by s ≈ 62°with respect to the ecliptic positions. The reactivity of 1 towards iodine and chalcogens E (E = S, Se, Te) was studied. Iodine reacts to give 1,1'-bis-[iodo(dimethyl)stannyl]ferrocene (6) and dimethyltin diiodide. In the case of the chalcogens, the detectable and isolated products are 1,3-distanna-2-chalcogena-[3]ferroceno-phanes (E = S (7), Se (8), Te ( )) in addition to trimeric dimethyltin chalcogenides, (Me 2 SnE) 3 . Crystals suitable for X-ray structural analysis could be obtained of 1,3-distanna-2thia-[3]ferrocenophane (7); the triclinic unit cell (space group P 1) has the dimensions a = 6.538( ), b = 9.013(2), c = 15.442(2) A Ê ; α = 92.15(2), b = 91.89(2), c = 109.43(2)°. The molecular structures of 1 and 7 are compared with those of other 1,3-distanna-[3]ferrocenophanes. All compounds were studied by NMR spectroscopy ( 1 H, 13 C, 77 Se, 119 Sn and 125 Te NMR) in order to establish the presence of the [3]ferrocenophanes 7±9 and of the cycles (Me 2 SnE) 3 in solution.