K3YbB2(PO7)2 crystallizes in the trigonal R-3 space group. There are two inequivalent K sites. In the first K site, K(1) is bonded in an octahedral geometry to six equivalent O(3) atoms. In the second K site, K(2) is bonded in a 9-coordinate geometry to three equivalent O(3) and six equivalent O(1) atoms. Yb(1) is bonded to six equivalent O(1) atoms to form YbO6 octahedra that share corners with six equivalent P(1)O4 tetrahedra. B(1) is bonded in a trigonal planar geometry to three equivalent O(3) atoms. P(1) is bonded to one O(2) and three equivalent O(1) atoms to form PO4 tetrahedra that share corners with three equivalent Yb(1)O6 octahedra. The corner-sharing octahedral tilt angles are 18°. There are three inequivalent O sites. In the first O site, O(3) is bonded in a distorted single-bond geometry to one K(1), one K(2), and one B(1) atom. In the second O site, O(1) is bonded in a 2-coordinate geometry to two equivalent K(2), one Yb(1), and one P(1) atom. In the third O site, O(2) is bonded in a single-bond geometry to one P(1) atom.
K3YbB2(PO7)2 crystallizes in the trigonal R-3 space group. There are two inequivalent K sites. In the first K site, K(1) is bonded in an octahedral geometry to six equivalent O(3) atoms. All K(1)-O(3) bond lengths are 2.79 Å. In the second K site, K(2) is bonded in a 9-coordinate geometry to three equivalent O(3) and six equivalent O(1) atoms. All K(2)-O(3) bond lengths are 2.86 Å. There are three shorter (3.04 Å) and three longer (3.12 Å) K(2)-O(1) bond lengths. Yb(1) is bonded to six equivalent O(1) atoms to form YbO6 octahedra that share corners with six equivalent P(1)O4 tetrahedra. All Yb(1)-O(1) bond lengths are 2.28 Å. B(1) is bonded in a trigonal planar geometry to three equivalent O(3) atoms. All B(1)-O(3) bond lengths are 1.37 Å. P(1) is bonded to one O(2) and three equivalent O(1) atoms to form PO4 tetrahedra that share corners with three equivalent Yb(1)O6 octahedra. The corner-sharing octahedral tilt angles are 18°. The P(1)-O(2) bond length is 1.59 Å. All P(1)-O(1) bond lengths are 1.54 Å. There are three inequivalent O sites. In the first O site, O(3) is bonded in a distorted single-bond geometry to one K(1), one K(2), and one B(1) atom. In the second O site, O(1) is bonded in a 2-coordinate geometry to two equivalent K(2), one Yb(1), and one P(1) atom. In the third O site, O(2) is bonded in a single-bond geometry to one P(1) atom.