Trimeric,cyclic Ti10-containing 27-tungsto-3-germanate [(α-Ti3GeW9O37OH)3(TiO3(OH2)3)]17−

The trimeric, cyclic polyanion [(α-Ti₃GeW₉O₃₇OH)₃(TiO₃(OH₂)₃)]^17? (Ti₁₀) was synthesized by reaction of [A-α-GeW₉O₃₄]^10? with K₈[Ti₄O₄(C₂O₄)₈] in a mixture of rubidium and lithium acetate buffers at 60 °C, and then crystallized as a mixed rubidium-potassium-sodium salt, Rb₁₃K₂Na₂[(α-Ti₃GeW₉O₃₇OH)₃(TiO₃(OH₂)₃)]·40H₂O (Rb-Ti₁₀). The title compound was characterized in the solid state by IR, single-crystal XRD, TGA and elemental analysis, and in solution by ¹⁸³W-NMR. In order to prepare a pure sample of Rb-Ti₁₀, several reaction parameters need to be carefully controlled, such as the ratio of rubidium and lithium acetate buffers, the choice of titanium precursor (K₈[Ti₄O₄(C₂O₄)₈]), the reaction temperature, and very importantly, the concentration of rubidium ions.     

Complexes of Ge(IV)- and Sn(IV)-fluorides with cyclic and acyclic carbenes: bis(dialkylamino)-difluoromethylenes as carbene sources

Carbene complexes of Ge(IV)- and Sn(IV)-fluorides have been synthesized by oxidative addition of 2,2-difluoro-1,3-dimethylimidazolidine and bis(dimethylamino)difluoromethane to GeCl(2)?dioxane and SnF(2). Chloride analogs of the Ge(IV) complexes were also isolated. All compounds were characterized in the solid state by single-crystal X-ray diffraction.