Ti13S24 crystallizes in the triclinic P-1 space group. There are eight inequivalent Ti sites. In the first Ti site, Ti(1) is bonded to one S(1), one S(11), one S(5), one S(7), and two equivalent S(9) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. In the second Ti site, Ti(2) is bonded to one S(12), one S(2), one S(6), one S(8), and two equivalent S(10) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. In the third Ti site, Ti(3) is bonded to one S(1), one S(12), one S(3), one S(4), one S(5), and one S(8) atom to form a mixture of edge and face-sharing TiS6 octahedra. In the fourth Ti site, Ti(4) is bonded to two equivalent S(4), two equivalent S(5), and two equivalent S(8) atoms to form a mixture of face and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles range from 48-49°. In the fifth Ti site, Ti(5) is bonded to one S(11), one S(2), one S(3), one S(4), one S(6), and one S(7) atom to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 49°. In the sixth Ti site, Ti(6) is bonded to two equivalent S(1), two equivalent S(4), and two equivalent S(7) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. In the seventh Ti site, Ti(7) is bonded to two equivalent S(2), two equivalent S(3), and two equivalent S(8) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. In the eighth Ti site, Ti(8) is bonded to one S(10), one S(11), one S(12), one S(5), one S(6), and one S(9) atom to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. There are twelve inequivalent S sites. In the first S site, S(1) is bonded in a distorted T-shaped geometry to one Ti(1), one Ti(3), and one Ti(6) atom. In the second S site, S(2) is bonded in a distorted T-shaped geometry to one Ti(2), one Ti(5), and one Ti(7) atom. In the third S site, S(3) is bonded in a distorted T-shaped geometry to one Ti(3), one Ti(5), and one Ti(7) atom. In the fourth S site, S(4) is bonded in a rectangular see-saw-like geometry to one Ti(3), one Ti(4), one Ti(5), and one Ti(6) atom. In the fifth S site, S(5) is bonded in a rectangular see-saw-like geometry to one Ti(1), one Ti(3), one Ti(4), and one Ti(8) atom. In the sixth S site, S(6) is bonded in a distorted T-shaped geometry to one Ti(2), one Ti(5), and one Ti(8) atom. In the seventh S site, S(7) is bonded in a distorted T-shaped geometry to one Ti(1), one Ti(5), and one Ti(6) atom. In the eighth S site, S(8) is bonded in a rectangular see-saw-like geometry to one Ti(2), one Ti(3), one Ti(4), and one Ti(7) atom. In the ninth S site, S(9) is bonded in a distorted T-shaped geometry to one Ti(8) and two equivalent Ti(1) atoms. In the tenth S site, S(10) is bonded in a distorted T-shaped geometry to one Ti(8) and two equivalent Ti(2) atoms. In the eleventh S site, S(11) is bonded in a distorted T-shaped geometry to one Ti(1), one Ti(5), and one Ti(8) atom. In the twelfth S site, S(12) is bonded in a distorted T-shaped geometry to one Ti(2), one Ti(3), and one Ti(8) atom.
Ti13S24 crystallizes in the triclinic P-1 space group. There are eight inequivalent Ti sites. In the first Ti site, Ti(1) is bonded to one S(1), one S(11), one S(5), one S(7), and two equivalent S(9) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. The Ti(1)-S(1) bond length is 2.43 Å. The Ti(1)-S(11) bond length is 2.36 Å. The Ti(1)-S(5) bond length is 2.54 Å. The Ti(1)-S(7) bond length is 2.40 Å. There is one shorter (2.42 Å) and one longer (2.44 Å) Ti(1)-S(9) bond length. In the second Ti site, Ti(2) is bonded to one S(12), one S(2), one S(6), one S(8), and two equivalent S(10) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. The Ti(2)-S(12) bond length is 2.41 Å. The Ti(2)-S(2) bond length is 2.43 Å. The Ti(2)-S(6) bond length is 2.45 Å. The Ti(2)-S(8) bond length is 2.50 Å. There is one shorter (2.39 Å) and one longer (2.41 Å) Ti(2)-S(10) bond length. In the third Ti site, Ti(3) is bonded to one S(1), one S(12), one S(3), one S(4), one S(5), and one S(8) atom to form a mixture of edge and face-sharing TiS6 octahedra. The Ti(3)-S(1) bond length is 2.40 Å. The Ti(3)-S(12) bond length is 2.42 Å. The Ti(3)-S(3) bond length is 2.42 Å. The Ti(3)-S(4) bond length is 2.47 Å. The Ti(3)-S(5) bond length is 2.47 Å. The Ti(3)-S(8) bond length is 2.49 Å. In the fourth Ti site, Ti(4) is bonded to two equivalent S(4), two equivalent S(5), and two equivalent S(8) atoms to form a mixture of face and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles range from 48-49°. Both Ti(4)-S(4) bond lengths are 2.46 Å. Both Ti(4)-S(5) bond lengths are 2.46 Å. Both Ti(4)-S(8) bond lengths are 2.46 Å. In the fifth Ti site, Ti(5) is bonded to one S(11), one S(2), one S(3), one S(4), one S(6), and one S(7) atom to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 49°. The Ti(5)-S(11) bond length is 2.44 Å. The Ti(5)-S(2) bond length is 2.39 Å. The Ti(5)-S(3) bond length is 2.41 Å. The Ti(5)-S(4) bond length is 2.53 Å. The Ti(5)-S(6) bond length is 2.38 Å. The Ti(5)-S(7) bond length is 2.44 Å. In the sixth Ti site, Ti(6) is bonded to two equivalent S(1), two equivalent S(4), and two equivalent S(7) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. Both Ti(6)-S(1) bond lengths are 2.42 Å. Both Ti(6)-S(4) bond lengths are 2.46 Å. Both Ti(6)-S(7) bond lengths are 2.41 Å. In the seventh Ti site, Ti(7) is bonded to two equivalent S(2), two equivalent S(3), and two equivalent S(8) atoms to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. Both Ti(7)-S(2) bond lengths are 2.41 Å. Both Ti(7)-S(3) bond lengths are 2.43 Å. Both Ti(7)-S(8) bond lengths are 2.46 Å. In the eighth Ti site, Ti(8) is bonded to one S(10), one S(11), one S(12), one S(5), one S(6), and one S(9) atom to form a mixture of edge and corner-sharing TiS6 octahedra. The corner-sharing octahedral tilt angles are 48°. The Ti(8)-S(10) bond length is 2.43 Å. The Ti(8)-S(11) bond length is 2.44 Å. The Ti(8)-S(12) bond length is 2.42 Å. The Ti(8)-S(5) bond length is 2.51 Å. The Ti(8)-S(6) bond length is 2.39 Å. The Ti(8)-S(9) bond length is 2.41 Å. There are twelve inequivalent S sites. In the first S site, S(1) is bonded in a distorted T-shaped geometry to one Ti(1), one Ti(3), and one Ti(6) atom. In the second S site, S(2) is bonded in a distorted T-shaped geometry to one Ti(2), one Ti(5), and one Ti(7) atom. In the third S site, S(3) is bonded in a distorted T-shaped geometry to one Ti(3), one Ti(5), and one Ti(7) atom. In the fourth S site, S(4) is bonded in a rectangular see-saw-like geometry to one Ti(3), one Ti(4), one Ti(5), and one Ti(6) atom. In the fifth S site, S(5) is bonded in a rectangular see-saw-like geometry to one Ti(1), one Ti(3), one Ti(4), and one Ti(8) atom. In the sixth S site, S(6) is bonded in a distorted T-shaped geometry to one Ti(2), one Ti(5), and one Ti(8) atom. In the seventh S site, S(7) is bonded in a distorted T-shaped geometry to one Ti(1), one Ti(5), and one Ti(6) atom. In the eighth S site, S(8) is bonded in a rectangular see-saw-like geometry to one Ti(2), one Ti(3), one Ti(4), and one Ti(7) atom. In the ninth S site, S(9) is bonded in a distorted T-shaped geometry to one Ti(8) and two equivalent Ti(1) atoms. In the tenth S site, S(10) is bonded in a distorted T-shaped geometry to one Ti(8) and two equivalent Ti(2) atoms. In the eleventh S site, S(11) is bonded in a distorted T-shaped geometry to one Ti(1), one Ti(5), and one Ti(8) atom. In the twelfth S site, S(12) is bonded in a distorted T-shaped geometry to one Ti(2), one Ti(3), and one Ti(8) atom.