The synthesis and complete characterization by multinuclear NMR, infrared, and Mössbauer spectroscopy, by single crystal X-ray analysis, as well as by electrospray mass spectrometry of the new soluble triorganotin fluoride Me 2 PhSnF (1)

Reactions in solution of the hypercoordinated organotin chlorides {2,6-[P(O)(OEt) 2 ] 2 -4-t-Bu-C 6 H 2 }SnCl 2 X (X ) Ph, Cl) with fluoride ions have been studied using temperaturedependent 119 Sn and 31 P NMR spectroscopy and electrospray mass spectrometry. The syntheses and molecular structures of the novel intramolecularly coordinated diorganotin difluoride {2,6- 3), and the monoorganotin difluoride hydroxide {{2,6-[P(O)(OEt) 2 ] 2 -4-t-Bu-C 6 H 2 }SnF 2 OH} 2 (6) are reported. In the crystal lattice, compound 1 forms an adduct composed of two tin moieties and a water molecule which are linked via F‚‚‚H-O-H‚‚‚F hydrogen bridges. The intramolecularly coordinated benzoxaphosphastannole derivative 3 is formed by intramolecular cyclization of {2,6-[P(O)(OEt) 2 ] 2 -4-t-Bu-C 6 H 2 }SnCl 2 Ph with elimination of ethyl chloride and dimerization. The organotin difluoride hydroxide derivative 6 is a dimer in the solid state as a result of intermolecular hydroxide bridges. Also present are intramolecular Sn-O-H‚‚‚OdP hydrogen bonds. The configuration at tin is best described as a monocapped octahedron.

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The syntheses of 1,1′-bis(chloromethyldimethylsilyl)ferrocene, fc(SiMe 2 CH 2 Cl) 2 (2), of the series of open-chain ferrocene-and silicon-containing organotin(IV) compounds 14), and of the ferrocenophanesPh) are reported, and the molecular structures of 4, 16, 17, 19, 20, 22, and 23 are described. In solution, the halogen-substituted ferrocenophanes 17-19 undergo cis-trans isomerization, the rate of which is enhanced by addition of halide ions. Variable-temperature 119 Sn and 19 F NMR studies in solution indicate that the fluoro derivatives 9, 13, and 18 react with different molar equivalents of fluoride ions to give the 1:1 and 1:2 adductsrespectively. A more extended electrochemical investigation points out that the species containing halogen-substituted tin groups are more sensitive to anions than their analogues containing diphenyltin groups.

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