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Hexamethyl‐1,2,3‐tristanna‐[3]ferrocenophane – Molecular Structure and Cleavage of the Tin–Tin Bonds by Iodine, Sulfur, Selenium, and Tellurium
Author(s) -
Herberhold Max,
Steffl Udo,
Milius Wolfgang,
Wrackmeyer Bernd
Publication year - 1998
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/(sici)1521-3749(199803)624:3<386::aid-zaac386>3.0.co;2-n
Subject(s) - triclinic crystal system , chalcogen , chemistry , crystallography , ferrocene , tellurium , cyclopentadienyl complex , monoclinic crystal system , molecule , tin , reactivity (psychology) , stereochemistry , crystal structure , inorganic chemistry , organic chemistry , catalysis , alternative medicine , electrode , pathology , electrochemistry , medicine
Hexamethyl‐1,2,3‐tristanna‐[3]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) Å; β = 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 τ £ 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]ferrocenophanes (E = S ( 7 ), Se ( 8 ), Te ( 9 )) in addition to trimeric dimethyltin chalcogenides, (Me 2 SnE) 3 . Crystals suitable for X‐ray structural analysis could be obtained of 1,3‐distanna‐2‐thia‐[3]ferrocenophane ( 7 ); the triclinic unit cell (space group P 1) has the dimensions a = 6.538(2), b = 9.013(2), c = 15.442(2) Å; α = 92.15(2), β = 91.89(2), γ = 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.