NaYbTiNbO6F crystallizes in the tetragonal P4_122 space group. Na(1) is bonded to two equivalent O(1), two equivalent O(2), two equivalent O(4), and two equivalent F(1) atoms to form distorted NaO6F2 hexagonal bipyramids that share edges with two equivalent Na(1)O6F2 hexagonal bipyramids, edges with four equivalent Yb(1)O6F2 hexagonal bipyramids, edges with two equivalent Ti(1)O6 octahedra, and edges with four equivalent Nb(1)O6 octahedra. Yb(1) is bonded to two equivalent O(1), two equivalent O(2), two equivalent O(3), and two equivalent F(1) atoms to form distorted YbO6F2 hexagonal bipyramids that share edges with two equivalent Yb(1)O6F2 hexagonal bipyramids, edges with four equivalent Na(1)O6F2 hexagonal bipyramids, edges with two equivalent Nb(1)O6 octahedra, and edges with four equivalent Ti(1)O6 octahedra. Ti(1) is bonded to two equivalent O(1), two equivalent O(2), and two equivalent O(3) atoms to form TiO6 octahedra that share corners with two equivalent Ti(1)O6 octahedra, corners with four equivalent Nb(1)O6 octahedra, edges with two equivalent Na(1)O6F2 hexagonal bipyramids, and edges with four equivalent Yb(1)O6F2 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 44-45°. Nb(1) is bonded to two equivalent O(1), two equivalent O(2), and two equivalent O(4) atoms to form NbO6 octahedra that share corners with two equivalent Nb(1)O6 octahedra, corners with four equivalent Ti(1)O6 octahedra, edges with two equivalent Yb(1)O6F2 hexagonal bipyramids, and edges with four equivalent Na(1)O6F2 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 43-44°. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to one Na(1), one Yb(1), one Ti(1), and one Nb(1) atom. In the second O site, O(2) is bonded in a 4-coordinate geometry to one Na(1), one Yb(1), one Ti(1), and one Nb(1) atom. In the third O site, O(3) is bonded in a 4-coordinate geometry to two equivalent Yb(1) and two equivalent Ti(1) atoms. In the fourth O site, O(4) is bonded in a 4-coordinate geometry to two equivalent Na(1) and two equivalent Nb(1) atoms. F(1) is bonded to two equivalent Na(1) and two equivalent Yb(1) atoms to form corner-sharing FNa2Yb2 tetrahedra.
NaYbTiNbO6F crystallizes in the tetragonal P4_122 space group. Na(1) is bonded to two equivalent O(1), two equivalent O(2), two equivalent O(4), and two equivalent F(1) atoms to form distorted NaO6F2 hexagonal bipyramids that share edges with two equivalent Na(1)O6F2 hexagonal bipyramids, edges with four equivalent Yb(1)O6F2 hexagonal bipyramids, edges with two equivalent Ti(1)O6 octahedra, and edges with four equivalent Nb(1)O6 octahedra. Both Na(1)-O(1) bond lengths are 2.66 Å. Both Na(1)-O(2) bond lengths are 2.69 Å. Both Na(1)-O(4) bond lengths are 2.63 Å. Both Na(1)-F(1) bond lengths are 2.29 Å. Yb(1) is bonded to two equivalent O(1), two equivalent O(2), two equivalent O(3), and two equivalent F(1) atoms to form distorted YbO6F2 hexagonal bipyramids that share edges with two equivalent Yb(1)O6F2 hexagonal bipyramids, edges with four equivalent Na(1)O6F2 hexagonal bipyramids, edges with two equivalent Nb(1)O6 octahedra, and edges with four equivalent Ti(1)O6 octahedra. Both Yb(1)-O(1) bond lengths are 2.54 Å. Both Yb(1)-O(2) bond lengths are 2.53 Å. Both Yb(1)-O(3) bond lengths are 2.61 Å. Both Yb(1)-F(1) bond lengths are 2.21 Å. Ti(1) is bonded to two equivalent O(1), two equivalent O(2), and two equivalent O(3) atoms to form TiO6 octahedra that share corners with two equivalent Ti(1)O6 octahedra, corners with four equivalent Nb(1)O6 octahedra, edges with two equivalent Na(1)O6F2 hexagonal bipyramids, and edges with four equivalent Yb(1)O6F2 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 44-45°. Both Ti(1)-O(1) bond lengths are 1.98 Å. Both Ti(1)-O(2) bond lengths are 1.95 Å. Both Ti(1)-O(3) bond lengths are 1.95 Å. Nb(1) is bonded to two equivalent O(1), two equivalent O(2), and two equivalent O(4) atoms to form NbO6 octahedra that share corners with two equivalent Nb(1)O6 octahedra, corners with four equivalent Ti(1)O6 octahedra, edges with two equivalent Yb(1)O6F2 hexagonal bipyramids, and edges with four equivalent Na(1)O6F2 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 43-44°. Both Nb(1)-O(1) bond lengths are 1.98 Å. Both Nb(1)-O(2) bond lengths are 2.00 Å. Both Nb(1)-O(4) bond lengths are 2.01 Å. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to one Na(1), one Yb(1), one Ti(1), and one Nb(1) atom. In the second O site, O(2) is bonded in a 4-coordinate geometry to one Na(1), one Yb(1), one Ti(1), and one Nb(1) atom. In the third O site, O(3) is bonded in a 4-coordinate geometry to two equivalent Yb(1) and two equivalent Ti(1) atoms. In the fourth O site, O(4) is bonded in a 4-coordinate geometry to two equivalent Na(1) and two equivalent Nb(1) atoms. F(1) is bonded to two equivalent Na(1) and two equivalent Yb(1) atoms to form corner-sharing FNa2Yb2 tetrahedra.