RbYb(WO4)2 crystallizes in the monoclinic C2/c space group. Rb(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 in a 6-coordinate geometry to two equivalent O(2), two equivalent O(3), and two equivalent O(4) atoms. W(1) is bonded to one O(2), one O(4), two equivalent O(1), and two equivalent O(3) atoms to form a mixture of corner and edge-sharing WO6 octahedra. The corner-sharing octahedral tilt angles are 42°. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent Rb(1) and two equivalent W(1) atoms. In the second O site, O(2) is bonded in a 2-coordinate geometry to one Rb(1), one Yb(1), and one W(1) atom. In the third O site, O(3) is bonded in a 4-coordinate geometry to one Rb(1), one Yb(1), and two equivalent W(1) atoms. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Rb(1), one Yb(1), and one W(1) atom.
RbYb(WO4)2 crystallizes in the monoclinic C2/c space group. Rb(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 Rb(1)-O(2) bond lengths are 3.10 Å. Both Rb(1)-O(3) bond lengths are 3.06 Å. Both Rb(1)-O(4) bond lengths are 2.91 Å. There are two shorter (2.98 Å) and two longer (3.03 Å) Rb(1)-O(1) bond lengths. Yb(1) is bonded in a 6-coordinate geometry to two equivalent O(2), two equivalent O(3), and two equivalent O(4) atoms. Both Yb(1)-O(2) bond lengths are 2.39 Å. Both Yb(1)-O(3) bond lengths are 2.34 Å. Both Yb(1)-O(4) bond lengths are 2.34 Å. W(1) is bonded to one O(2), one O(4), two equivalent O(1), and two equivalent O(3) atoms to form a mixture of corner and edge-sharing WO6 octahedra. The corner-sharing octahedral tilt angles are 42°. The W(1)-O(2) bond length is 1.84 Å. The W(1)-O(4) bond length is 1.83 Å. There is one shorter (1.90 Å) and one longer (2.11 Å) W(1)-O(1) bond length. There is one shorter (2.02 Å) and one longer (2.12 Å) W(1)-O(3) 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 Rb(1) and two equivalent W(1) atoms. In the second O site, O(2) is bonded in a 2-coordinate geometry to one Rb(1), one Yb(1), and one W(1) atom. In the third O site, O(3) is bonded in a 4-coordinate geometry to one Rb(1), one Yb(1), and two equivalent W(1) atoms. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Rb(1), one Yb(1), and one W(1) atom.