An organic-inorganic hybrid polyoxoniobate, Na 8 {Ni[Ni(en)] 2 Nb 10 O 32 }$28H 2 O (1) (en ¼ ethanediamine), has been synthesized and characterized. It represents the first example of a trinuclear nickel-containing polyoxoniobate. The catalysis of 1 for allylic alcohol epoxidation was investigated at room temperature in aqueous solution, and was found to catalyze the epoxidation of 3-methyl-2-buten-1-ol with high conversion (98%) and selectivity (94%). Furthermore, magnetic measurements showed that the compound exhibits ferromagnetic interactions. † Electronic supplementary information (ESI) available: Bond valence sum calculations of O and Ni (Tables S1 and S2), additional structural gures ( Fig. S1 and S2), additional measurements ( Fig. S3-S8, Tables S3 and S4), catalytic properties (Fig. S9, S10, Tables S5 and S6). CCDC 1526285 for 1. For ESI and crystallographic data in CIF or other electronic format see a Conversion determined by GC with dodecane as an internal standard. The products were identied by GC-MS. b Reaction conditions for the entries 1 to 5: catalyst (12 mmol), substrate (5 mmol) and H 2 O (3 mL) at 25 C. c Blank experiment, the reaction was carried out without catalyst. d Reaction conditions: catalyst (6 mmol), substrate (5 mmol) and H 2 O (3 mL) at 25 C. e Reaction conditions for the entries 7 to 10: catalyst (12 mmol), substrate (5 mmol) and H 2 O (3 mL) at 35 C. f cis-and trans-mixture.This journal is

A gigantic 16-copper-containing 28-niobate cluster, Na K H {As Cu [Cu(H O)] Nb O }⋅37.5 H O (1), has been prepared by a one-pot reaction, which is the first example of arsenic copper clusters containing polyoxoniobate, and the first tetrahedral arrangement of both the Cu cluster and the [Nb O ] subunits.

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