NH 4 ) 2 [B 2 P 3 O 11 (OH)] was synthesized as a crystalline colorless powder by reaction of (NH 4 ) 2 HPO 4 , H 3 BO 3 , and H 3 PO 4 under hydrothermal conditions at 180°C. According to X-ray single-crystal investigations (NH 4 ) 2 [B 2 P 3 O 11 (OH)] crystallizes in a new structure type in the orthorhombic space group P2 1 2 1 2 1 (no. 19) [Z = 4, a = 4.509(3), b = 14.490(11), c = 16.401(12) Å, R 1 = 0.046, wR 2 = 0.093, 1682 data, 200 parameters]. The crystal structure comprises infinite