Synthesis and Crystal Structure of a Novel Layered Barium Antimonate Ba 2Sb7O13(OH) with Mixed-Valence Antimony. -Pale brown crystals of Ba 2Sb7O13(OH) are prepared by hydrothermal reaction of Ba(OH)2, Sb2O3, KCl, and H2O (autoclave, 190 C, 4 d). The compound crystallizes in the trigonal space group P3 (Z = 1, single crystal XRD) and represents a novel layered structure composed of corner-sharing Sb V O6 and Sb III O4 polyhedra. DFT calculations as well as optical diffuse reflectance spectroscopy measurements indicate that the compound is an indirect band semiconductor with an optical band gap of 2.7 eV. -(GENG*, L.; MENG, C.-Y.; WANG, M.-M.; DAI, K.; LIN, C.-S.; CHENG, W.-D.; Solid State Sci. 44 (2015) 27-31, http://dx.