KYb(WO4)2 crystallizes in the monoclinic C2/c space group. K(1) is bonded in a 10-coordinate geometry to two equivalent O(2), two equivalent O(3), two equivalent O(4), and four equivalent O(1) atoms. Yb(1) is bonded to two equivalent O(2), two equivalent O(3), and two equivalent O(4) atoms to form distorted YbO6 pentagonal pyramids that share corners with eight equivalent W(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 26-61°. W(1) is bonded to one O(2), one O(3), two equivalent O(1), and two equivalent O(4) atoms to form WO6 octahedra that share corners with two equivalent W(1)O6 octahedra, corners with four equivalent Yb(1)O6 pentagonal pyramids, and  an edgeedge with one W(1)O6 octahedra. The corner-sharing octahedral tilt angles are 38°. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent K(1) and two equivalent W(1) atoms. In the second O site, O(2) is bonded in a 2-coordinate geometry to one K(1), one Yb(1), and one W(1) atom. In the third O site, O(3) is bonded in a 3-coordinate geometry to one K(1), one Yb(1), and one W(1) atom. In the fourth O site, O(4) is bonded to one K(1), one Yb(1), and two equivalent W(1) atoms to form a mixture of distorted corner and edge-sharing OKYbW2 tetrahedra.
KYb(WO4)2 crystallizes in the monoclinic C2/c space group. K(1) is bonded in a 10-coordinate geometry to two equivalent O(2), two equivalent O(3), two equivalent O(4), and four equivalent O(1) atoms. Both K(1)-O(2) bond lengths are 2.99 Å. Both K(1)-O(3) bond lengths are 2.86 Å. Both K(1)-O(4) bond lengths are 2.95 Å. There are two shorter (2.92 Å) and two longer (3.15 Å) K(1)-O(1) bond lengths. Yb(1) is bonded to two equivalent O(2), two equivalent O(3), and two equivalent O(4) atoms to form distorted YbO6 pentagonal pyramids that share corners with eight equivalent W(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 26-61°. Both Yb(1)-O(2) bond lengths are 2.33 Å. Both Yb(1)-O(3) bond lengths are 2.32 Å. Both Yb(1)-O(4) bond lengths are 2.34 Å. W(1) is bonded to one O(2), one O(3), two equivalent O(1), and two equivalent O(4) atoms to form WO6 octahedra that share corners with two equivalent W(1)O6 octahedra, corners with four equivalent Yb(1)O6 pentagonal pyramids, and  an edgeedge with one W(1)O6 octahedra. The corner-sharing octahedral tilt angles are 38°. The W(1)-O(2) bond length is 1.84 Å. The W(1)-O(3) bond length is 1.83 Å. There is one shorter (1.96 Å) and one longer (2.00 Å) W(1)-O(1) bond length. There is one shorter (2.04 Å) and one longer (2.10 Å) W(1)-O(4) bond length. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent K(1) and two equivalent W(1) atoms. In the second O site, O(2) is bonded in a 2-coordinate geometry to one K(1), one Yb(1), and one W(1) atom. In the third O site, O(3) is bonded in a 3-coordinate geometry to one K(1), one Yb(1), and one W(1) atom. In the fourth O site, O(4) is bonded to one K(1), one Yb(1), and two equivalent W(1) atoms to form a mixture of distorted corner and edge-sharing OKYbW2 tetrahedra.