KHo(WO4)2 crystallizes in the monoclinic C2/c space group. K(1) is bonded in a 10-coordinate geometry to two equivalent O(1), two equivalent O(3), two equivalent O(4), and four equivalent O(2) atoms. Ho(1) is bonded in a 6-coordinate geometry to two equivalent O(1), two equivalent O(3), and two equivalent O(4) atoms. W(1) is bonded to one O(3), one O(4), two equivalent O(1), and two equivalent O(2) atoms to form a mixture of corner and edge-sharing WO6 octahedra. The corner-sharing octahedral tilt angles are 43°. There are four inequivalent O sites. In the first O site, O(1) is bonded to one K(1), one Ho(1), and two equivalent W(1) atoms to form distorted OKHoW2 tetrahedra that share corners with two equivalent O(1)KHoW2 tetrahedra, corners with four equivalent O(2)K2W2 trigonal pyramids,  an edgeedge with one O(1)KHoW2 tetrahedra, and edges with two equivalent O(2)K2W2 trigonal pyramids. In the second O site, O(2) is bonded to two equivalent K(1) and two equivalent W(1) atoms to form distorted OK2W2 trigonal pyramids that share corners with four equivalent O(1)KHoW2 tetrahedra, corners with six equivalent O(2)K2W2 trigonal pyramids, edges with two equivalent O(1)KHoW2 tetrahedra, and  an edgeedge with one O(2)K2W2 trigonal pyramid. In the third O site, O(3) is bonded in a 3-coordinate geometry to one K(1), one Ho(1), and one W(1) atom. In the fourth O site, O(4) is bonded in a 2-coordinate geometry to one K(1), one Ho(1), and one W(1) atom.
KHo(WO4)2 crystallizes in the monoclinic C2/c space group. K(1) is bonded in a 10-coordinate geometry to two equivalent O(1), two equivalent O(3), two equivalent O(4), and four equivalent O(2) atoms. Both K(1)-O(1) bond lengths are 3.00 Å. Both K(1)-O(3) bond lengths are 2.86 Å. Both K(1)-O(4) bond lengths are 3.11 Å. There are two shorter (2.88 Å) and two longer (2.94 Å) K(1)-O(2) bond lengths. Ho(1) is bonded in a 6-coordinate geometry to two equivalent O(1), two equivalent O(3), and two equivalent O(4) atoms. Both Ho(1)-O(1) bond lengths are 2.29 Å. Both Ho(1)-O(3) bond lengths are 2.26 Å. Both Ho(1)-O(4) bond lengths are 2.30 Å. W(1) is bonded to one O(3), one O(4), two equivalent O(1), and two equivalent O(2) atoms to form a mixture of corner and edge-sharing WO6 octahedra. The corner-sharing octahedral tilt angles are 43°. The W(1)-O(3) bond length is 1.83 Å. The W(1)-O(4) bond length is 1.85 Å. There is one shorter (2.02 Å) and one longer (2.12 Å) W(1)-O(1) bond length. There is one shorter (1.88 Å) and one longer (2.13 Å) W(1)-O(2) bond length. There are four inequivalent O sites. In the first O site, O(1) is bonded to one K(1), one Ho(1), and two equivalent W(1) atoms to form distorted OKHoW2 tetrahedra that share corners with two equivalent O(1)KHoW2 tetrahedra, corners with four equivalent O(2)K2W2 trigonal pyramids,  an edgeedge with one O(1)KHoW2 tetrahedra, and edges with two equivalent O(2)K2W2 trigonal pyramids. In the second O site, O(2) is bonded to two equivalent K(1) and two equivalent W(1) atoms to form distorted OK2W2 trigonal pyramids that share corners with four equivalent O(1)KHoW2 tetrahedra, corners with six equivalent O(2)K2W2 trigonal pyramids, edges with two equivalent O(1)KHoW2 tetrahedra, and  an edgeedge with one O(2)K2W2 trigonal pyramid. In the third O site, O(3) is bonded in a 3-coordinate geometry to one K(1), one Ho(1), and one W(1) atom. In the fourth O site, O(4) is bonded in a 2-coordinate geometry to one K(1), one Ho(1), and one W(1) atom.