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61.
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. 相似文献
62.
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. 相似文献