Mo13O33 crystallizes in the triclinic P1 space group. There are thirteen inequivalent Mo sites. In the first Mo site, Mo(1) is bonded to one O(12), one O(14), one O(15), one O(23), and two equivalent O(5) atoms to form corner-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 2-13°. In the second Mo site, Mo(2) is bonded to one O(11), one O(13), one O(16), one O(23), and two equivalent O(6) atoms to form corner-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 1-9°. In the third Mo site, Mo(3) is bonded to one O(11), one O(17), one O(28), one O(3), and two equivalent O(8) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 0-33°. In the fourth Mo site, Mo(4) is bonded to one O(12), one O(18), one O(29), one O(4), and two equivalent O(7) atoms to form a mixture of distorted corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 4-33°. In the fifth Mo site, Mo(5) is bonded to one O(13), one O(19), one O(24), one O(30), and two equivalent O(2) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 6-32°. In the sixth Mo site, Mo(6) is bonded to one O(14), one O(20), one O(25), one O(31), and two equivalent O(1) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 2-31°. In the seventh Mo site, Mo(7) is bonded to one O(21), one O(25), one O(26), one O(7), and two equivalent O(18) atoms to form MoO6 octahedra that share  a cornercorner with one Mo(11)O6 octahedra,  a cornercorner with one Mo(6)O6 octahedra, corners with two equivalent Mo(7)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(4)O6 octahedra. The corner-sharing octahedral tilt angles range from 0-32°. In the eighth Mo site, Mo(8) is bonded to one O(22), one O(24), one O(27), one O(8), and two equivalent O(17) atoms to form distorted MoO6 octahedra that share  a cornercorner with one Mo(12)O6 octahedra,  a cornercorner with one Mo(5)O6 octahedra, corners with two equivalent Mo(8)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 3-33°. In the ninth Mo site, Mo(9) is bonded to one O(1), one O(19), one O(3), one O(9), and two equivalent O(31) atoms to form distorted MoO6 octahedra that share  a cornercorner with one Mo(3)O6 octahedra,  a cornercorner with one Mo(5)O6 octahedra, corners with two equivalent Mo(9)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(6)O6 octahedra. The corner-sharing octahedral tilt angles range from 6-31°. In the tenth Mo site, Mo(10) is bonded to one O(10), one O(2), one O(20), one O(4), and two equivalent O(30) atoms to form distorted MoO6 octahedra that share  a cornercorner with one Mo(4)O6 octahedra,  a cornercorner with one Mo(6)O6 octahedra, corners with two equivalent Mo(10)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(5)O6 octahedra. The corner-sharing octahedral tilt angles range from 3-32°. In the eleventh Mo site, Mo(11) is bonded to one O(15), one O(21), one O(28), one O(32), and two equivalent O(33) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 0-26°. In the twelfth Mo site, Mo(12) is bonded to one O(16), one O(22), one O(29), one O(33), and two equivalent O(32) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 1-28°. In the thirteenth Mo site, Mo(13) is bonded to one O(10), one O(26), one O(27), and one O(9) atom to form corner-sharing MoO4 tetrahedra. The corner-sharing octahedral tilt angles range from 45-47°. There are thirty-three inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal non-coplanar geometry to one Mo(9) and two equivalent Mo(6) atoms. In the second O site, O(2) is bonded in a distorted trigonal non-coplanar geometry to one Mo(10) and two equivalent Mo(5) atoms. In the third O site, O(3) is bonded in a linear geometry to one Mo(3) and one Mo(9) atom. In the fourth O site, O(4) is bonded in a linear geometry to one Mo(10) and one Mo(4) atom. In the fifth O site, O(5) is bonded in a linear geometry to two equivalent Mo(1) atoms. In the sixth O site, O(6) is bonded in a linear geometry to two equivalent Mo(2) atoms. In the seventh O site, O(7) is bonded in a distorted trigonal non-coplanar geometry to one Mo(7) and two equivalent Mo(4) atoms. In the eighth O site, O(8) is bonded in a distorted trigonal non-coplanar geometry to one Mo(8) and two equivalent Mo(3) atoms. In the ninth O site, O(9) is bonded in a distorted bent 120 degrees geometry to one Mo(13) and one Mo(9) atom. In the tenth O site, O(10) is bonded in a distorted bent 120 degrees geometry to one Mo(10) and one Mo(13) atom. In the eleventh O site, O(11) is bonded in a linear geometry to one Mo(2) and one Mo(3) atom. In the twelfth O site, O(12) is bonded in a linear geometry to one Mo(1) and one Mo(4) atom. In the thirteenth O site, O(13) is bonded in a linear geometry to one Mo(2) and one Mo(5) atom. In the fourteenth O site, O(14) is bonded in a linear geometry to one Mo(1) and one Mo(6) atom. In the fifteenth O site, O(15) is bonded in a linear geometry to one Mo(1) and one Mo(11) atom. In the sixteenth O site, O(16) is bonded in a linear geometry to one Mo(12) and one Mo(2) atom. In the seventeenth O site, O(17) is bonded in a distorted trigonal non-coplanar geometry to one Mo(3) and two equivalent Mo(8) atoms. In the eighteenth O site, O(18) is bonded in a distorted trigonal non-coplanar geometry to one Mo(4) and two equivalent Mo(7) atoms. In the nineteenth O site, O(19) is bonded in a linear geometry to one Mo(5) and one Mo(9) atom. In the twentieth O site, O(20) is bonded in a linear geometry to one Mo(10) and one Mo(6) atom. In the twenty-first O site, O(21) is bonded in a linear geometry to one Mo(11) and one Mo(7) atom. In the twenty-second O site, O(22) is bonded in a linear geometry to one Mo(12) and one Mo(8) atom. In the twenty-third O site, O(23) is bonded in a linear geometry to one Mo(1) and one Mo(2) atom. In the twenty-fourth O site, O(24) is bonded in a linear geometry to one Mo(5) and one Mo(8) atom. In the twenty-fifth O site, O(25) is bonded in a linear geometry to one Mo(6) and one Mo(7) atom. In the twenty-sixth O site, O(26) is bonded in a distorted bent 150 degrees geometry to one Mo(13) and one Mo(7) atom. In the twenty-seventh O site, O(27) is bonded in a distorted bent 120 degrees geometry to one Mo(13) and one Mo(8) atom. In the twenty-eighth O site, O(28) is bonded in a linear geometry to one Mo(11) and one Mo(3) atom. In the twenty-ninth O site, O(29) is bonded in a linear geometry to one Mo(12) and one Mo(4) atom. In the thirtieth O site, O(30) is bonded in a distorted trigonal non-coplanar geometry to one Mo(5) and two equivalent Mo(10) atoms. In the thirty-first O site, O(31) is bonded in a distorted trigonal non-coplanar geometry to one Mo(6) and two equivalent Mo(9) atoms. In the thirty-second O site, O(32) is bonded in a distorted T-shaped geometry to one Mo(11) and two equivalent Mo(12) atoms. In the thirty-third O site, O(33) is bonded in a distorted T-shaped geometry to one Mo(12) and two equivalent Mo(11) atoms.
Mo13O33 crystallizes in the triclinic P1 space group. There are thirteen inequivalent Mo sites. In the first Mo site, Mo(1) is bonded to one O(12), one O(14), one O(15), one O(23), and two equivalent O(5) atoms to form corner-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 2-13°. The Mo(1)-O(12) bond length is 2.23 Å. The Mo(1)-O(14) bond length is 2.07 Å. The Mo(1)-O(15) bond length is 1.82 Å. The Mo(1)-O(23) bond length is 1.84 Å. There is one shorter (1.92 Å) and one longer (2.01 Å) Mo(1)-O(5) bond length. In the second Mo site, Mo(2) is bonded to one O(11), one O(13), one O(16), one O(23), and two equivalent O(6) atoms to form corner-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 1-9°. The Mo(2)-O(11) bond length is 2.18 Å. The Mo(2)-O(13) bond length is 2.10 Å. The Mo(2)-O(16) bond length is 1.90 Å. The Mo(2)-O(23) bond length is 2.02 Å. There is one shorter (1.95 Å) and one longer (1.96 Å) Mo(2)-O(6) bond length. In the third Mo site, Mo(3) is bonded to one O(11), one O(17), one O(28), one O(3), and two equivalent O(8) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 0-33°. The Mo(3)-O(11) bond length is 1.77 Å. The Mo(3)-O(17) bond length is 2.18 Å. The Mo(3)-O(28) bond length is 1.96 Å. The Mo(3)-O(3) bond length is 2.10 Å. There is one shorter (2.03 Å) and one longer (2.04 Å) Mo(3)-O(8) bond length. In the fourth Mo site, Mo(4) is bonded to one O(12), one O(18), one O(29), one O(4), and two equivalent O(7) atoms to form a mixture of distorted corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 4-33°. The Mo(4)-O(12) bond length is 1.77 Å. The Mo(4)-O(18) bond length is 2.19 Å. The Mo(4)-O(29) bond length is 1.95 Å. The Mo(4)-O(4) bond length is 2.10 Å. There is one shorter (2.03 Å) and one longer (2.04 Å) Mo(4)-O(7) bond length. In the fifth Mo site, Mo(5) is bonded to one O(13), one O(19), one O(24), one O(30), and two equivalent O(2) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 6-32°. The Mo(5)-O(13) bond length is 1.78 Å. The Mo(5)-O(19) bond length is 1.92 Å. The Mo(5)-O(24) bond length is 2.13 Å. The Mo(5)-O(30) bond length is 2.19 Å. There is one shorter (2.01 Å) and one longer (2.05 Å) Mo(5)-O(2) bond length. In the sixth Mo site, Mo(6) is bonded to one O(14), one O(20), one O(25), one O(31), and two equivalent O(1) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 2-31°. The Mo(6)-O(14) bond length is 1.83 Å. The Mo(6)-O(20) bond length is 1.95 Å. The Mo(6)-O(25) bond length is 2.09 Å. The Mo(6)-O(31) bond length is 2.21 Å. There is one shorter (1.99 Å) and one longer (2.06 Å) Mo(6)-O(1) bond length. In the seventh Mo site, Mo(7) is bonded to one O(21), one O(25), one O(26), one O(7), and two equivalent O(18) atoms to form MoO6 octahedra that share  a cornercorner with one Mo(11)O6 octahedra,  a cornercorner with one Mo(6)O6 octahedra, corners with two equivalent Mo(7)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(4)O6 octahedra. The corner-sharing octahedral tilt angles range from 0-32°. The Mo(7)-O(21) bond length is 1.93 Å. The Mo(7)-O(25) bond length is 1.80 Å. The Mo(7)-O(26) bond length is 2.12 Å. The Mo(7)-O(7) bond length is 2.17 Å. There is one shorter (2.03 Å) and one longer (2.04 Å) Mo(7)-O(18) bond length. In the eighth Mo site, Mo(8) is bonded to one O(22), one O(24), one O(27), one O(8), and two equivalent O(17) atoms to form distorted MoO6 octahedra that share  a cornercorner with one Mo(12)O6 octahedra,  a cornercorner with one Mo(5)O6 octahedra, corners with two equivalent Mo(8)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 3-33°. The Mo(8)-O(22) bond length is 1.90 Å. The Mo(8)-O(24) bond length is 1.79 Å. The Mo(8)-O(27) bond length is 2.13 Å. The Mo(8)-O(8) bond length is 2.17 Å. There is one shorter (2.03 Å) and one longer (2.04 Å) Mo(8)-O(17) bond length. In the ninth Mo site, Mo(9) is bonded to one O(1), one O(19), one O(3), one O(9), and two equivalent O(31) atoms to form distorted MoO6 octahedra that share  a cornercorner with one Mo(3)O6 octahedra,  a cornercorner with one Mo(5)O6 octahedra, corners with two equivalent Mo(9)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(6)O6 octahedra. The corner-sharing octahedral tilt angles range from 6-31°. The Mo(9)-O(1) bond length is 2.21 Å. The Mo(9)-O(19) bond length is 1.91 Å. The Mo(9)-O(3) bond length is 1.80 Å. The Mo(9)-O(9) bond length is 2.12 Å. There is one shorter (1.99 Å) and one longer (2.07 Å) Mo(9)-O(31) bond length. In the tenth Mo site, Mo(10) is bonded to one O(10), one O(2), one O(20), one O(4), and two equivalent O(30) atoms to form distorted MoO6 octahedra that share  a cornercorner with one Mo(4)O6 octahedra,  a cornercorner with one Mo(6)O6 octahedra, corners with two equivalent Mo(10)O6 octahedra,  a cornercorner with one Mo(13)O4 tetrahedra, and edges with two equivalent Mo(5)O6 octahedra. The corner-sharing octahedral tilt angles range from 3-32°. The Mo(10)-O(10) bond length is 2.14 Å. The Mo(10)-O(2) bond length is 2.19 Å. The Mo(10)-O(20) bond length is 1.88 Å. The Mo(10)-O(4) bond length is 1.80 Å. There is one shorter (2.00 Å) and one longer (2.06 Å) Mo(10)-O(30) bond length. In the eleventh Mo site, Mo(11) is bonded to one O(15), one O(21), one O(28), one O(32), and two equivalent O(33) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 0-26°. The Mo(11)-O(15) bond length is 2.02 Å. The Mo(11)-O(21) bond length is 1.89 Å. The Mo(11)-O(28) bond length is 1.89 Å. The Mo(11)-O(32) bond length is 2.10 Å. Both Mo(11)-O(33) bond lengths are 2.00 Å. In the twelfth Mo site, Mo(12) is bonded to one O(16), one O(22), one O(29), one O(33), and two equivalent O(32) atoms to form a mixture of corner and edge-sharing MoO6 octahedra. The corner-sharing octahedral tilt angles range from 1-28°. The Mo(12)-O(16) bond length is 1.92 Å. The Mo(12)-O(22) bond length is 1.92 Å. The Mo(12)-O(29) bond length is 1.89 Å. The Mo(12)-O(33) bond length is 2.13 Å. Both Mo(12)-O(32) bond lengths are 2.01 Å. In the thirteenth Mo site, Mo(13) is bonded to one O(10), one O(26), one O(27), and one O(9) atom to form corner-sharing MoO4 tetrahedra. The corner-sharing octahedral tilt angles range from 45-47°. The Mo(13)-O(10) bond length is 1.79 Å. The Mo(13)-O(26) bond length is 1.79 Å. The Mo(13)-O(27) bond length is 1.79 Å. The Mo(13)-O(9) bond length is 1.79 Å. There are thirty-three inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal non-coplanar geometry to one Mo(9) and two equivalent Mo(6) atoms. In the second O site, O(2) is bonded in a distorted trigonal non-coplanar geometry to one Mo(10) and two equivalent Mo(5) atoms. In the third O site, O(3) is bonded in a linear geometry to one Mo(3) and one Mo(9) atom. In the fourth O site, O(4) is bonded in a linear geometry to one Mo(10) and one Mo(4) atom. In the fifth O site, O(5) is bonded in a linear geometry to two equivalent Mo(1) atoms. In the sixth O site, O(6) is bonded in a linear geometry to two equivalent Mo(2) atoms. In the seventh O site, O(7) is bonded in a distorted trigonal non-coplanar geometry to one Mo(7) and two equivalent Mo(4) atoms. In the eighth O site, O(8) is bonded in a distorted trigonal non-coplanar geometry to one Mo(8) and two equivalent Mo(3) atoms. In the ninth O site, O(9) is bonded in a distorted bent 120 degrees geometry to one Mo(13) and one Mo(9) atom. In the tenth O site, O(10) is bonded in a distorted bent 120 degrees geometry to one Mo(10) and one Mo(13) atom. In the eleventh O site, O(11) is bonded in a linear geometry to one Mo(2) and one Mo(3) atom. In the twelfth O site, O(12) is bonded in a linear geometry to one Mo(1) and one Mo(4) atom. In the thirteenth O site, O(13) is bonded in a linear geometry to one Mo(2) and one Mo(5) atom. In the fourteenth O site, O(14) is bonded in a linear geometry to one Mo(1) and one Mo(6) atom. In the fifteenth O site, O(15) is bonded in a linear geometry to one Mo(1) and one Mo(11) atom. In the sixteenth O site, O(16) is bonded in a linear geometry to one Mo(12) and one Mo(2) atom. In the seventeenth O site, O(17) is bonded in a distorted trigonal non-coplanar geometry to one Mo(3) and two equivalent Mo(8) atoms. In the eighteenth O site, O(18) is bonded in a distorted trigonal non-coplanar geometry to one Mo(4) and two equivalent Mo(7) atoms. In the nineteenth O site, O(19) is bonded in a linear geometry to one Mo(5) and one Mo(9) atom. In the twentieth O site, O(20) is bonded in a linear geometry to one Mo(10) and one Mo(6) atom. In the twenty-first O site, O(21) is bonded in a linear geometry to one Mo(11) and one Mo(7) atom. In the twenty-second O site, O(22) is bonded in a linear geometry to one Mo(12) and one Mo(8) atom. In the twenty-third O site, O(23) is bonded in a linear geometry to one Mo(1) and one Mo(2) atom. In the twenty-fourth O site, O(24) is bonded in a linear geometry to one Mo(5) and one Mo(8) atom. In the twenty-fifth O site, O(25) is bonded in a linear geometry to one Mo(6) and one Mo(7) atom. In the twenty-sixth O site, O(26) is bonded in a distorted bent 150 degrees geometry to one Mo(13) and one Mo(7) atom. In the twenty-seventh O site, O(27) is bonded in a distorted bent 120 degrees geometry to one Mo(13) and one Mo(8) atom. In the twenty-eighth O site, O(28) is bonded in a linear geometry to one Mo(11) and one Mo(3) atom. In the twenty-ninth O site, O(29) is bonded in a linear geometry to one Mo(12) and one Mo(4) atom. In the thirtieth O site, O(30) is bonded in a distorted trigonal non-coplanar geometry to one Mo(5) and two equivalent Mo(10) atoms. In the thirty-first O site, O(31) is bonded in a distorted trigonal non-coplanar geometry to one Mo(6) and two equivalent Mo(9) atoms. In the thirty-second O site, O(32) is bonded in a distorted T-shaped geometry to one Mo(11) and two equivalent Mo(12) atoms. In the thirty-third O site, O(33) is bonded in a distorted T-shaped geometry to one Mo(12) and two equivalent Mo(11) atoms.