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Li7Ta24O64 crystallizes in the monoclinic Pm space group. The structure is three-dimensional. there are seven inequivalent Li sites. In the first Li site, Li is bonded in a 4-coordinate geometry to six O atoms. There are a spread of Li–O bond distances ranging from 2.13–2.61 Å. In the second Li site, Li is bonded in a 4-coordinate geometry to four O atoms. There are a spread of Li–O bond distances ranging from 2.13–2.49 Å. In the third Li site, Li is bonded in a 4-coordinate geometry to four O atoms. There are a spread of Li–O bond distances ranging from 2.15–2.43 Å. In the fourth Li site, Li is bonded in a 4-coordinate geometry to four O atoms. There are a spread of Li–O bond distances ranging from 2.13–2.48 Å. In the fifth Li site, Li is bonded in a 5-coordinate geometry to five O atoms. There are a spread of Li–O bond distances ranging from 1.90–2.33 Å. In the sixth Li site, Li is bonded in a 5-coordinate geometry to five O atoms. There are a spread of Li–O bond distances ranging from 1.89–2.35 Å. In the seventh Li site, Li is bonded in a 3-coordinate geometry to seven O atoms. There are a spread of Li–O bond distances ranging from 1.99–2.60 Å. There are twelve inequivalent Ta sites. In the first Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 12–39°. There are a spread of Ta–O bond distances ranging from 1.93–2.09 Å. In the second Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 16–38°. There are a spread of Ta–O bond distances ranging from 1.91–2.16 Å. In the third Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 14–38°. There are a spread of Ta–O bond distances ranging from 1.94–2.09 Å. In the fourth Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 16–38°. There are a spread of Ta–O bond distances ranging from 1.92–2.16 Å. In the fifth Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 17–39°. There are a spread of Ta–O bond distances ranging from 1.94–2.06 Å. In the sixth Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 17–38°. There are a spread of Ta–O bond distances ranging from 1.94–2.06 Å. In the seventh Ta site, Ta is bonded to seven O atoms to form TaO7 pentagonal bipyramids that share corners with two equivalent TaO7 pentagonal bipyramids and edges with five TaO6 octahedra. There are a spread of Ta–O bond distances ranging from 1.93–2.14 Å. In the eighth Ta site, Ta is bonded to seven O atoms to form TaO7 pentagonal bipyramids that share corners with two equivalent TaO7 pentagonal bipyramids and edges with five TaO6 octahedra. There are a spread of Ta–O bond distances ranging from 1.93–2.15 Å. In the ninth Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 1–37°. There are a spread of Ta–O bond distances ranging from 1.93–2.13 Å. In the tenth Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 0–38°. There are a spread of Ta–O bond distances ranging from 1.91–2.10 Å. In the eleventh Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 1–38°. There are a spread of Ta–O bond distances ranging from 1.94–2.10 Å. In the twelfth Ta site, Ta is bonded to six O atoms to form TaO6 octahedra that share corners with six TaO6 octahedra and an edgeedge with one TaO7 pentagonal bipyramid. The corner-sharing octahedra tilt angles range from 0–38°. There are a spread of Ta–O bond distances ranging from 1.92–2.09 Å. There are forty-four inequivalent O sites. In the first O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the second O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the third O site, O is bonded in a distorted trigonal non-coplanar geometry to three Ta atoms. In the fourth O site, O is bonded in a distorted trigonal non-coplanar geometry to three Ta atoms. In the fifth O site, O is bonded in a distorted trigonal non-coplanar geometry to three Ta atoms. In the sixth O site, O is bonded in a distorted trigonal non-coplanar geometry to three Ta atoms. In the seventh O site, O is bonded in a distorted trigonal planar geometry to one Li and two Ta atoms. In the eighth O site, O is bonded in a bent 150 degrees geometry to two Ta atoms. In the ninth O site, O is bonded in a distorted bent 150 degrees geometry to one Li and two Ta atoms. In the tenth O site, O is bonded in a bent 150 degrees geometry to two Ta atoms. In the eleventh O site, O is bonded in a distorted T-shaped geometry to two Li and two equivalent Ta atoms. In the twelfth O site, O is bonded in a T-shaped geometry to one Li and two equivalent Ta atoms. In the thirteenth O site, O is bonded in a T-shaped geometry to one Li and two equivalent Ta atoms. In the fourteenth O site, O is bonded in a T-shaped geometry to one Li and two equivalent Ta atoms. In the fifteenth O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the sixteenth O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the seventeenth O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the eighteenth O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the nineteenth O site, O is bonded in a distorted trigonal non-coplanar geometry to three Ta atoms. In the twentieth O site, O is bonded in a distorted trigonal planar geometry to three Ta atoms. In the twenty-first O site, O is bonded in a distorted trigonal non-coplanar geometry to three Ta atoms. In the twenty-second O site, O is bonded in a distorted trigonal planar geometry to three Ta atoms. In the twenty-third O site, O is bonded to one Li and three Ta atoms to form distorted corner-sharing OLiTa3 tetrahedra. In the twenty-fourth O site, O is bonded to one Li and three Ta atoms to form distorted corner-sharing OLiTa3 tetrahedra. In the twenty-fifth O site, O is bonded in a 4-coordinate geometry to two Li and two equivalent Ta atoms. In the twenty-sixth O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the twenty-seventh O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the twenty-eighth O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the twenty-ninth O site, O is bonded in a distorted trigonal non-coplanar geometry to one Li and two Ta atoms. In the thirtieth O site, O is bonded in a distorted trigonal non-coplanar geometry to one Li and two Ta atoms. In the thirty-first O site, O is bonded in a distorted trigonal non-coplanar geometry to one Li and two Ta atoms. In the thirty-second O site, O is bonded in a distorted trigonal non-coplanar geometry to one Li and two Ta atoms. In the thirty-third O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the thirty-fourth O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the thirty-fifth O site, O is bonded in a bent 150 degrees geometry to two equivalent Ta atoms. In the thirty-sixth O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the thirty-seventh O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the thirty-eighth O site, O is bonded in a linear geometry to two equivalent Ta atoms. In the thirty-ninth O site, O is bonded in a T-shaped geometry to one Li and two equivalent Ta atoms. In the fortieth O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the forty-first O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the forty-second O site, O is bonded in a distorted T-shaped geometry to one Li and two equivalent Ta atoms. In the forty-third O site, O is bonded in a distorted linear geometry to one Li and two Ta atoms. In the forty-fourth O site, O is bonded in a distorted linear geometry to two Ta atoms.

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