The reaction of the incompletely condensed silsesquioxane (c-C5H9)7Si7O9(OH)3 with [Pd(C6H3Me2-2,4)(I)(bpy)] produced a complex with a Pd-O bond, [Pd(C6H3Me2-2,4){(c-C5H9)7Si7O10(OH)2}(bpy)]. Palladium complexes having a silsesquioxanate ligand, [Pd(Ar){R7Si7O10(OH)2}(tmeda)] (Ar = C6H5, C6F5, C6H3F2-2,4; R = c-C5H9, i-C4H9), were prepared by the reaction of the silsesquioxane R7Si7O9(OH)3 with arylpalladium iodo complexes, [Pd(Ar)(I)(tmeda)] (tmeda = N,N,N',N'-tetramethylethylenediamine), in the presence of Ag2O. These complexes were characterized by multinuclear (1H, 13C{1H}, 19F{1H}, and 29Si{1H}) NMR spectroscopy, and the structure of [Pd(C6F5){(c-C5H9)7Si7O10(OH)2}(tmeda)] was determined by X-ray crystallography. Temperature-dependent 1H and 19F{1H} NMR spectra revealed the dynamic behavior of the complexes on the NMR time scale.
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