CaYb4Ti2O10 crystallizes in the triclinic P1 space group. Ca(1) is bonded in a 6-coordinate geometry to one O(1), one O(10), one O(3), one O(4), one O(5), and one O(9) atom. There are four inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to one O(1), one O(2), one O(3), one O(4), one O(7), and one O(8) atom to form distorted YbO6 pentagonal pyramids that share corners with two equivalent Yb(2)O6 pentagonal pyramids, corners with three equivalent Ti(2)O5 trigonal bipyramids, and edges with two equivalent Ti(1)O6 octahedra. In the second Yb site, Yb(2) is bonded to one O(10), one O(2), one O(5), one O(6), one O(7), and one O(9) atom to form distorted YbO6 pentagonal pyramids that share corners with two equivalent Ti(1)O6 octahedra, corners with two equivalent Yb(1)O6 pentagonal pyramids,  an edgeedge with one Ti(1)O6 octahedra, and  an edgeedge with one Ti(2)O5 trigonal bipyramid. The corner-sharing octahedral tilt angles range from 20-39°. In the third Yb site, Yb(3) is bonded in a 6-coordinate geometry to one O(2), one O(3), one O(4), one O(6), one O(7), and one O(8) atom. In the fourth Yb site, Yb(4) is bonded in a 6-coordinate geometry to one O(10), one O(2), one O(5), one O(6), one O(7), and one O(9) atom. There are two inequivalent Ti sites. In the first Ti site, Ti(1) is bonded to one O(10), one O(2), one O(3), one O(6), one O(7), and one O(8) atom to form TiO6 octahedra that share corners with two equivalent Yb(2)O6 pentagonal pyramids,  a cornercorner with one Ti(2)O5 trigonal bipyramid,  an edgeedge with one Yb(2)O6 pentagonal pyramid, and edges with two equivalent Yb(1)O6 pentagonal pyramids. In the second Ti site, Ti(2) is bonded to one O(1), one O(4), one O(5), one O(8), and one O(9) atom to form distorted TiO5 trigonal bipyramids that share  a cornercorner with one Ti(1)O6 octahedra, corners with three equivalent Yb(1)O6 pentagonal pyramids, and  an edgeedge with one Yb(2)O6 pentagonal pyramid. The corner-sharing octahedral tilt angles are 67°. There are ten inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one Ca(1), one Yb(1), and one Ti(2) atom. In the second O site, O(2) is bonded to one Yb(1), one Yb(2), one Yb(3), one Yb(4), and one Ti(1) atom to form distorted OYb4Ti square pyramids that share corners with two equivalent O(6)Yb3Ti tetrahedra,  a cornercorner with one O(7)Yb4Ti trigonal bipyramid, corners with two equivalent O(5)CaYb2Ti trigonal pyramids,  an edgeedge with one O(6)Yb3Ti tetrahedra, edges with two equivalent O(7)Yb4Ti trigonal bipyramids, and  an edgeedge with one O(4)CaYb2Ti trigonal pyramid. In the third O site, O(3) is bonded in a 4-coordinate geometry to one Ca(1), one Yb(1), one Yb(3), and one Ti(1) atom. In the fourth O site, O(4) is bonded to one Ca(1), one Yb(1), one Yb(3), and one Ti(2) atom to form distorted OCaYb2Ti trigonal pyramids that share  a cornercorner with one O(6)Yb3Ti tetrahedra, corners with two equivalent O(7)Yb4Ti trigonal bipyramids, corners with two equivalent O(5)CaYb2Ti trigonal pyramids, and  an edgeedge with one O(2)Yb4Ti square pyramid. In the fifth O site, O(5) is bonded to one Ca(1), one Yb(2), one Yb(4), and one Ti(2) atom to form distorted OCaYb2Ti trigonal pyramids that share corners with two equivalent O(2)Yb4Ti square pyramids, corners with two equivalent O(6)Yb3Ti tetrahedra, corners with two equivalent O(4)CaYb2Ti trigonal pyramids, and  an edgeedge with one O(7)Yb4Ti trigonal bipyramid. In the sixth O site, O(6) is bonded to one Yb(2), one Yb(3), one Yb(4), and one Ti(1) atom to form OYb3Ti tetrahedra that share corners with two equivalent O(2)Yb4Ti square pyramids,  a cornercorner with one O(4)CaYb2Ti trigonal pyramid, corners with two equivalent O(5)CaYb2Ti trigonal pyramids,  an edgeedge with one O(2)Yb4Ti square pyramid, and edges with two equivalent O(7)Yb4Ti trigonal bipyramids. In the seventh O site, O(7) is bonded to one Yb(1), one Yb(2), one Yb(3), one Yb(4), and one Ti(1) atom to form OYb4Ti trigonal bipyramids that share  a cornercorner with one O(2)Yb4Ti square pyramid, corners with two equivalent O(4)CaYb2Ti trigonal pyramids, edges with two equivalent O(2)Yb4Ti square pyramids, edges with two equivalent O(6)Yb3Ti tetrahedra, and  an edgeedge with one O(5)CaYb2Ti trigonal pyramid. In the eighth O site, O(8) is bonded in a distorted rectangular see-saw-like geometry to one Yb(1), one Yb(3), one Ti(1), and one Ti(2) atom. In the ninth O site, O(9) is bonded in a distorted see-saw-like geometry to one Ca(1), one Yb(2), one Yb(4), and one Ti(2) atom. In the tenth O site, O(10) is bonded in a 4-coordinate geometry to one Ca(1), one Yb(2), one Yb(4), and one Ti(1) atom.
CaYb4Ti2O10 crystallizes in the triclinic P1 space group. Ca(1) is bonded in a 6-coordinate geometry to one O(1), one O(10), one O(3), one O(4), one O(5), and one O(9) atom. The Ca(1)-O(1) bond length is 2.51 Å. The Ca(1)-O(10) bond length is 2.55 Å. The Ca(1)-O(3) bond length is 2.64 Å. The Ca(1)-O(4) bond length is 2.30 Å. The Ca(1)-O(5) bond length is 2.30 Å. The Ca(1)-O(9) bond length is 2.29 Å. There are four inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to one O(1), one O(2), one O(3), one O(4), one O(7), and one O(8) atom to form distorted YbO6 pentagonal pyramids that share corners with two equivalent Yb(2)O6 pentagonal pyramids, corners with three equivalent Ti(2)O5 trigonal bipyramids, and edges with two equivalent Ti(1)O6 octahedra. The Yb(1)-O(1) bond length is 2.39 Å. The Yb(1)-O(2) bond length is 2.40 Å. The Yb(1)-O(3) bond length is 2.23 Å. The Yb(1)-O(4) bond length is 2.30 Å. The Yb(1)-O(7) bond length is 2.51 Å. The Yb(1)-O(8) bond length is 2.50 Å. In the second Yb site, Yb(2) is bonded to one O(10), one O(2), one O(5), one O(6), one O(7), and one O(9) atom to form distorted YbO6 pentagonal pyramids that share corners with two equivalent Ti(1)O6 octahedra, corners with two equivalent Yb(1)O6 pentagonal pyramids,  an edgeedge with one Ti(1)O6 octahedra, and  an edgeedge with one Ti(2)O5 trigonal bipyramid. The corner-sharing octahedral tilt angles range from 20-39°. The Yb(2)-O(10) bond length is 2.44 Å. The Yb(2)-O(2) bond length is 2.35 Å. The Yb(2)-O(5) bond length is 2.29 Å. The Yb(2)-O(6) bond length is 2.17 Å. The Yb(2)-O(7) bond length is 2.44 Å. The Yb(2)-O(9) bond length is 2.33 Å. In the third Yb site, Yb(3) is bonded in a 6-coordinate geometry to one O(2), one O(3), one O(4), one O(6), one O(7), and one O(8) atom. The Yb(3)-O(2) bond length is 2.38 Å. The Yb(3)-O(3) bond length is 2.22 Å. The Yb(3)-O(4) bond length is 2.39 Å. The Yb(3)-O(6) bond length is 2.30 Å. The Yb(3)-O(7) bond length is 2.32 Å. The Yb(3)-O(8) bond length is 2.30 Å. In the fourth Yb site, Yb(4) is bonded in a 6-coordinate geometry to one O(10), one O(2), one O(5), one O(6), one O(7), and one O(9) atom. The Yb(4)-O(10) bond length is 2.45 Å. The Yb(4)-O(2) bond length is 2.42 Å. The Yb(4)-O(5) bond length is 2.31 Å. The Yb(4)-O(6) bond length is 2.18 Å. The Yb(4)-O(7) bond length is 2.31 Å. The Yb(4)-O(9) bond length is 2.28 Å. There are two inequivalent Ti sites. In the first Ti site, Ti(1) is bonded to one O(10), one O(2), one O(3), one O(6), one O(7), and one O(8) atom to form TiO6 octahedra that share corners with two equivalent Yb(2)O6 pentagonal pyramids,  a cornercorner with one Ti(2)O5 trigonal bipyramid,  an edgeedge with one Yb(2)O6 pentagonal pyramid, and edges with two equivalent Yb(1)O6 pentagonal pyramids. The Ti(1)-O(10) bond length is 2.01 Å. The Ti(1)-O(2) bond length is 1.92 Å. The Ti(1)-O(3) bond length is 1.94 Å. The Ti(1)-O(6) bond length is 1.93 Å. The Ti(1)-O(7) bond length is 2.04 Å. The Ti(1)-O(8) bond length is 2.12 Å. In the second Ti site, Ti(2) is bonded to one O(1), one O(4), one O(5), one O(8), and one O(9) atom to form distorted TiO5 trigonal bipyramids that share  a cornercorner with one Ti(1)O6 octahedra, corners with three equivalent Yb(1)O6 pentagonal pyramids, and  an edgeedge with one Yb(2)O6 pentagonal pyramid. The corner-sharing octahedral tilt angles are 67°. The Ti(2)-O(1) bond length is 1.94 Å. The Ti(2)-O(4) bond length is 2.08 Å. The Ti(2)-O(5) bond length is 1.88 Å. The Ti(2)-O(8) bond length is 1.88 Å. The Ti(2)-O(9) bond length is 1.85 Å. There are ten inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one Ca(1), one Yb(1), and one Ti(2) atom. In the second O site, O(2) is bonded to one Yb(1), one Yb(2), one Yb(3), one Yb(4), and one Ti(1) atom to form distorted OYb4Ti square pyramids that share corners with two equivalent O(6)Yb3Ti tetrahedra,  a cornercorner with one O(7)Yb4Ti trigonal bipyramid, corners with two equivalent O(5)CaYb2Ti trigonal pyramids,  an edgeedge with one O(6)Yb3Ti tetrahedra, edges with two equivalent O(7)Yb4Ti trigonal bipyramids, and  an edgeedge with one O(4)CaYb2Ti trigonal pyramid. In the third O site, O(3) is bonded in a 4-coordinate geometry to one Ca(1), one Yb(1), one Yb(3), and one Ti(1) atom. In the fourth O site, O(4) is bonded to one Ca(1), one Yb(1), one Yb(3), and one Ti(2) atom to form distorted OCaYb2Ti trigonal pyramids that share  a cornercorner with one O(6)Yb3Ti tetrahedra, corners with two equivalent O(7)Yb4Ti trigonal bipyramids, corners with two equivalent O(5)CaYb2Ti trigonal pyramids, and  an edgeedge with one O(2)Yb4Ti square pyramid. In the fifth O site, O(5) is bonded to one Ca(1), one Yb(2), one Yb(4), and one Ti(2) atom to form distorted OCaYb2Ti trigonal pyramids that share corners with two equivalent O(2)Yb4Ti square pyramids, corners with two equivalent O(6)Yb3Ti tetrahedra, corners with two equivalent O(4)CaYb2Ti trigonal pyramids, and  an edgeedge with one O(7)Yb4Ti trigonal bipyramid. In the sixth O site, O(6) is bonded to one Yb(2), one Yb(3), one Yb(4), and one Ti(1) atom to form OYb3Ti tetrahedra that share corners with two equivalent O(2)Yb4Ti square pyramids,  a cornercorner with one O(4)CaYb2Ti trigonal pyramid, corners with two equivalent O(5)CaYb2Ti trigonal pyramids,  an edgeedge with one O(2)Yb4Ti square pyramid, and edges with two equivalent O(7)Yb4Ti trigonal bipyramids. In the seventh O site, O(7) is bonded to one Yb(1), one Yb(2), one Yb(3), one Yb(4), and one Ti(1) atom to form OYb4Ti trigonal bipyramids that share  a cornercorner with one O(2)Yb4Ti square pyramid, corners with two equivalent O(4)CaYb2Ti trigonal pyramids, edges with two equivalent O(2)Yb4Ti square pyramids, edges with two equivalent O(6)Yb3Ti tetrahedra, and  an edgeedge with one O(5)CaYb2Ti trigonal pyramid. In the eighth O site, O(8) is bonded in a distorted rectangular see-saw-like geometry to one Yb(1), one Yb(3), one Ti(1), and one Ti(2) atom. In the ninth O site, O(9) is bonded in a distorted see-saw-like geometry to one Ca(1), one Yb(2), one Yb(4), and one Ti(2) atom. In the tenth O site, O(10) is bonded in a 4-coordinate geometry to one Ca(1), one Yb(2), one Yb(4), and one Ti(1) atom.