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The crystals of the title compound are hexagonal, space group  P 6 3 / mmc ,  a  = 13.852(2),  c  = 20.107(7) Å,  Z  = 2. 690 independent reflexions with  I  ≥ 3  σ  ( I ) were used for structure determination. The structure was solved by direct methods and refined by full-matrix least-squares to an  R  of 0.052. The cage anion [KV 15  O 36 ] 6−  is nearly spherical, having  D  3h  symmetry. Each vanadium atom is coordinated by five oxygen atoms to form a tetragonal pyramid. Fifteen pyramids are connected to each other via corners or edges of the basal planes. A large cavity in the center is about 4 Å in free diameter. The K +  ion is in the center of the cavity. The distances between K +  and 21 oxygen atoms located in the interior surface of the cavity are in the range of 3.33 – 3.87 Å and the distances between K +  and 15 V atoms are in the range of 3.32 – 3.53 Å. Six [(CH 3 ) 4 N] +  cations around the anion form a trigonal prism.

Synthesis and crystal structure of[(CH 3 ) 4 N] 6 [KV 15 O 36 ]