DOE OSTI2020
V9Sb7O32 is Hydrophilite-derived structured and crystallizes in the triclinic P-1 space group. The structure is three-dimensional. there are five inequivalent V+4.78+ sites. In the first V+4.78+ site, V+4.78+ is bonded to six O2- atoms to form VO6 octahedra that share corners with four VO6 octahedra, corners with four equivalent SbO6 octahedra, an edgeedge with one VO6 octahedra, and an edgeedge with one SbO6 octahedra. The corner-sharing octahedra tilt angles range from 49–53°. There are a spread of V–O bond distances ranging from 2.00–2.10 Å. In the second V+4.78+ site, V+4.78+ is bonded to six O2- atoms to form VO6 octahedra that share corners with four VO6 octahedra, corners with four SbO6 octahedra, and edges with two SbO6 octahedra. The corner-sharing octahedra tilt angles range from 49–53°. There are a spread of V–O bond distances ranging from 2.03–2.07 Å. In the third V+4.78+ site, V+4.78+ is bonded to six O2- atoms to form VO6 octahedra that share corners with four equivalent VO6 octahedra, corners with four equivalent SbO6 octahedra, and edges with two equivalent SbO6 octahedra. The corner-sharing octahedra tilt angles range from 50–52°. There are four shorter (2.03 Å) and two longer (2.06 Å) V–O bond lengths. In the fourth V+4.78+ site, V+4.78+ is bonded to six O2- atoms to form VO6 octahedra that share corners with two equivalent VO6 octahedra, corners with six SbO6 octahedra, an edgeedge with one VO6 octahedra, and an edgeedge with one SbO6 octahedra. The corner-sharing octahedra tilt angles range from 48–54°. There are a spread of V–O bond distances ranging from 1.98–2.09 Å. In the fifth V+4.78+ site, V+4.78+ is bonded to six O2- atoms to form VO6 octahedra that share corners with four VO6 octahedra, corners with four SbO6 octahedra, an edgeedge with one VO6 octahedra, and an edgeedge with one SbO6 octahedra. The corner-sharing octahedra tilt angles range from 47–52°. There are a spread of V–O bond distances ranging from 1.90–2.02 Å. There are four inequivalent Sb3+ sites. In the first Sb3+ site, Sb3+ is bonded to six O2- atoms to form SbO6 octahedra that share corners with two equivalent SbO6 octahedra, corners with six VO6 octahedra, and edges with two VO6 octahedra. The corner-sharing octahedra tilt angles range from 47–53°. There are a spread of Sb–O bond distances ranging from 1.99–2.04 Å. In the second Sb3+ site, Sb3+ is bonded to six O2- atoms to form SbO6 octahedra that share corners with two equivalent SbO6 octahedra, corners with six VO6 octahedra, an edgeedge with one VO6 octahedra, and an edgeedge with one SbO6 octahedra. The corner-sharing octahedra tilt angles range from 48–54°. There are a spread of Sb–O bond distances ranging from 1.98–2.06 Å. In the third Sb3+ site, Sb3+ is bonded to six O2- atoms to form SbO6 octahedra that share corners with two equivalent SbO6 octahedra, corners with six VO6 octahedra, and edges with two VO6 octahedra. The corner-sharing octahedra tilt angles range from 48–53°. There are a spread of Sb–O bond distances ranging from 1.98–2.04 Å. In the fourth Sb3+ site, Sb3+ is bonded to six O2- atoms to form SbO6 octahedra that share corners with four equivalent VO6 octahedra, corners with four equivalent SbO6 octahedra, and edges with two equivalent VO6 octahedra. The corner-sharing octahedra tilt angles range from 48–51°. There are two shorter (1.99 Å) and four longer (2.03 Å) Sb–O bond lengths. There are sixteen inequivalent O2- sites. In the first O2- site, O2- is bonded in a distorted trigonal planar geometry to one V+4.78+ and two Sb3+ atoms. In the second O2- site, O2- is bonded in a distorted trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the third O2- site, O2- is bonded in a distorted trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the fourth O2- site, O2- is bonded in a trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the fifth O2- site, O2- is bonded in a trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the sixth O2- site, O2- is bonded in a trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the seventh O2- site, O2- is bonded in a trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the eighth O2- site, O2- is bonded in a distorted trigonal planar geometry to one V+4.78+ and two Sb3+ atoms. In the ninth O2- site, O2- is bonded in a distorted trigonal planar geometry to one V+4.78+ and two Sb3+ atoms. In the tenth O2- site, O2- is bonded in a distorted trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the eleventh O2- site, O2- is bonded in a distorted trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the twelfth O2- site, O2- is bonded in a distorted trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the thirteenth O2- site, O2- is bonded in a distorted trigonal planar geometry to one V+4.78+ and two equivalent Sb3+ atoms. In the fourteenth O2- site, O2- is bonded in a distorted trigonal planar geometry to one V+4.78+ and two Sb3+ atoms. In the fifteenth O2- site, O2- is bonded in a distorted trigonal planar geometry to two V+4.78+ and one Sb3+ atom. In the sixteenth O2- site, O2- is bonded in a distorted trigonal planar geometry to two equivalent V+4.78+ and one Sb3+ atom.