PKU-6, a new aluminoborate (HAl
2B
3O
8), has been synthesizedin a closed system at 400
C. The structure of PKU-6, characterized by using powder and single-crystal X-ray diffraction, consistsof AlO
5 square-pyramidal chains and B
3O
7 groups, which areinterconnected and form a three-dimensional framework. The
27AlNMR study indicates that the isotropic chemical shift of pyramidalAl is 34.6 ppm with a large quadrupolar coupling constant (
CQ =4.2 MHz), mainly due to a nonspherical coordination environment.