TiSb3(PO4)6 crystallizes in the trigonal R3 space group. Ti(1) is bonded to three equivalent O(4) and three equivalent O(6) atoms to form TiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. There are three inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to three equivalent O(2) and three equivalent O(5) atoms to form SbO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. In the second Sb site, Sb(2) is bonded to three equivalent O(1) and three equivalent O(3) atoms to form SbO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. In the third Sb site, Sb(3) is bonded to three equivalent O(7) and three equivalent O(8) atoms to form SbO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. There are two inequivalent P sites. In the first P site, P(1) is bonded to one O(2), one O(3), one O(4), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one Ti(1)O6 octahedra,  a cornercorner with one Sb(1)O6 octahedra,  a cornercorner with one Sb(2)O6 octahedra, and  a cornercorner with one Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 21-35°. In the second P site, P(2) is bonded to one O(1), one O(5), one O(6), and one O(7) atom to form PO4 tetrahedra that share  a cornercorner with one Ti(1)O6 octahedra,  a cornercorner with one Sb(1)O6 octahedra,  a cornercorner with one Sb(2)O6 octahedra, and  a cornercorner with one Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 27-34°. There are eight inequivalent O sites. In the first O site, O(2) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(1) atom. In the second O site, O(3) is bonded in a bent 150 degrees geometry to one Sb(2) and one P(1) atom. In the third O site, O(4) is bonded in a bent 150 degrees geometry to one Ti(1) and one P(1) atom. In the fourth O site, O(5) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(2) atom. In the fifth O site, O(6) is bonded in a bent 150 degrees geometry to one Ti(1) and one P(2) atom. In the sixth O site, O(7) is bonded in a bent 150 degrees geometry to one Sb(3) and one P(2) atom. In the seventh O site, O(8) is bonded in a bent 150 degrees geometry to one Sb(3) and one P(1) atom. In the eighth O site, O(1) is bonded in a bent 150 degrees geometry to one Sb(2) and one P(2) atom.
TiSb3(PO4)6 crystallizes in the trigonal R3 space group. Ti(1) is bonded to three equivalent O(4) and three equivalent O(6) atoms to form TiO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. All Ti(1)-O(4) bond lengths are 2.00 Å. All Ti(1)-O(6) bond lengths are 1.93 Å. There are three inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to three equivalent O(2) and three equivalent O(5) atoms to form SbO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. All Sb(1)-O(2) bond lengths are 2.01 Å. All Sb(1)-O(5) bond lengths are 2.02 Å. In the second Sb site, Sb(2) is bonded to three equivalent O(1) and three equivalent O(3) atoms to form SbO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. All Sb(2)-O(1) bond lengths are 2.01 Å. All Sb(2)-O(3) bond lengths are 1.99 Å. In the third Sb site, Sb(3) is bonded to three equivalent O(7) and three equivalent O(8) atoms to form SbO6 octahedra that share corners with three equivalent P(1)O4 tetrahedra and corners with three equivalent P(2)O4 tetrahedra. All Sb(3)-O(7) bond lengths are 2.01 Å. All Sb(3)-O(8) bond lengths are 2.02 Å. There are two inequivalent P sites. In the first P site, P(1) is bonded to one O(2), one O(3), one O(4), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one Ti(1)O6 octahedra,  a cornercorner with one Sb(1)O6 octahedra,  a cornercorner with one Sb(2)O6 octahedra, and  a cornercorner with one Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 21-35°. The P(1)-O(2) bond length is 1.55 Å. The P(1)-O(3) bond length is 1.56 Å. The P(1)-O(4) bond length is 1.52 Å. The P(1)-O(8) bond length is 1.55 Å. In the second P site, P(2) is bonded to one O(1), one O(5), one O(6), and one O(7) atom to form PO4 tetrahedra that share  a cornercorner with one Ti(1)O6 octahedra,  a cornercorner with one Sb(1)O6 octahedra,  a cornercorner with one Sb(2)O6 octahedra, and  a cornercorner with one Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 27-34°. The P(2)-O(1) bond length is 1.56 Å. The P(2)-O(5) bond length is 1.55 Å. The P(2)-O(6) bond length is 1.53 Å. The P(2)-O(7) bond length is 1.54 Å. There are eight inequivalent O sites. In the first O site, O(2) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(1) atom. In the second O site, O(3) is bonded in a bent 150 degrees geometry to one Sb(2) and one P(1) atom. In the third O site, O(4) is bonded in a bent 150 degrees geometry to one Ti(1) and one P(1) atom. In the fourth O site, O(5) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(2) atom. In the fifth O site, O(6) is bonded in a bent 150 degrees geometry to one Ti(1) and one P(2) atom. In the sixth O site, O(7) is bonded in a bent 150 degrees geometry to one Sb(3) and one P(2) atom. In the seventh O site, O(8) is bonded in a bent 150 degrees geometry to one Sb(3) and one P(1) atom. In the eighth O site, O(1) is bonded in a bent 150 degrees geometry to one Sb(2) and one P(2) atom.