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Lanthanide (Ln)-containing polyoxometalates (POMs) have attracted particular attention owing to their structural diversity and potential applications in luminescence, magnetism, and catalysis. Herein three types of Ln-containing tungstotellurates(VI) (Ln = Dy 3+ , Ho 3+ , Er 3+ , Tm 3+ , Yb 3+ , and Lu 3+ ), dimeric (DMAH)  n  [H 22− n  {Ln(H 2 O) 3 [TeW 17 O 61 ]} 2 ] · mH 2 O (abbreviated as {Ln 2 Te 2 W 34 }; DMAH +  = dimethylammonium), mono-substituted (DMAH) 7 Na 2 {H 2 Ln(H 2 O) 4 [TeW 17 O 61 ]} · mH 2 O (abbreviated as {LnTeW 17 }), and three-dimensional (3D) inorganic frameworks (DMAH)  n  {H 3− n  Ln(H 2 O) 4 [TeW 6 O 24 ]} · mH 2 O (abbreviated as {LnTeW 6 }), have been synthesized by using simple metal salts and characterized by single-crystal X-ray diffraction and other routine techniques. Interestingly, the assembly of these POMs is pH dependent. Using the same starting materials, {Ln 2 Te 2 W 34 } were obtained at pH 1.7, where two Dawson-like monovacant [TeW 17 O 61 ] 14−  are linked by two Ln 3+  ions; mono-substituted Dawson-like {LnTeW 17 } were isolated at pH 1.9, and 3D inorganic framework {LnTeW 6 } based on Anderson-type [TeW 6 O 24 ] 6−  were formed at pH 2.3. It was also found that the assembly of Ln-containing POMs depends on the type of Ln 3+  ions. The three types of POMs can be prepared by using Ln 3+  ions with a relatively smaller ionic radius, such as Tb 3+ -Lu 3+ , while the use of Ln 3+  ions (La 3+ -Eu 3+ ) results in the formation of precipitation or {TeW 18 O 62 } clusters. Furthermore, three {LnTeW 6 } (Ln = Tb 3+ , Er 3+ , Lu 3+ ) were used as Lewis acid catalysts for the cyanosilylation of benzaldehydes, and their catalytic activity decreases with the decrease of Ln 3+  ionic radius, giving the order: {TbTeW 6 } > {ErTeW 6 } > {LuTeW 6 }. Notably, {TbTeW 6 } is stable to leaching and can be reused for five cycles without a significant loss of its activity.

Assembly of Lanthanide-Containing Tungstotellurates(VI): Syntheses, Structures, and Catalytic Properties