Abstract
Abstract : Crystalline complexes of 1,10-dichloro-1,10-distannabicyclo.8. 8hexacosane and benzyltriphenylphosphonium chloride (complex 3) and of 1,8- dichloro-1,8-distannabicyclo-6.6.6eicosane and tetrabutylammonium fluoride (complex 4) have been studied by X ray crystallography and solid state 119 Sn NMR spectroscopy. The halide ions are encrypted within the cavities of the bicyclic hosts in both complexes. Complex 3 is a stannates stannane species wherein one of the Lewis acidic tins binds the chloride strongly and the other interacts with the chloride only weakly. Complex 4 is a bis-hemistannate species wherein the Lewis acidic tin atoms bind the guest fluoride simultaneously. Low temperature species wherein the Lewis acidic tin the two complexes in halogenated solvents were studied. A chloride jump from one tin to the other was observed in complex 3; the dynamic process has an activation energy of 5.3 kcal/ mol. Line broadening of the tin signals in complex 4 was consistent with a similar fluoride jump with an activation energy of 2.9 kcal/mol. The crystalline complexes were reasonable models for the solution complexes in both cases, and the structural features in the solid state can be used to rationalize the binding in solution.
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