Mo12Co3(P2O13)4 crystallizes in the triclinic P-1 space group. There are six inequivalent Mo sites. In the first Mo site, Mo(1) is bonded to one O(12), one O(22), one O(26), one O(6), and one O(9) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Co(2)O6 octahedra,  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra,  an edgeedge with one Mo(5)O5 square pyramid, and  an edgeedge with one Mo(6)O5 square pyramid. The corner-sharing octahedral tilt angles are 45°. The Mo(1)-O(12) bond length is 2.29 Å. The Mo(1)-O(22) bond length is 1.94 Å. The Mo(1)-O(26) bond length is 1.99 Å. The Mo(1)-O(6) bond length is 2.05 Å. The Mo(1)-O(9) bond length is 2.08 Å. In the second Mo site, Mo(2) is bonded to one O(11), one O(15), one O(16), one O(21), and one O(25) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Co(2)O6 octahedra,  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra,  an edgeedge with one Mo(3)O5 square pyramid, and  an edgeedge with one Mo(4)O5 square pyramid. The corner-sharing octahedral tilt angles are 46°. The Mo(2)-O(11) bond length is 2.32 Å. The Mo(2)-O(15) bond length is 2.05 Å. The Mo(2)-O(16) bond length is 2.07 Å. The Mo(2)-O(21) bond length is 1.95 Å. The Mo(2)-O(25) bond length is 1.98 Å. In the third Mo site, Mo(3) is bonded to one O(13), one O(19), one O(20), one O(21), and one O(25) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Co(2)O6 octahedra,  a cornercorner with one P(3)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra,  an edgeedge with one Mo(2)O5 square pyramid, and  an edgeedge with one Mo(5)O5 square pyramid. The corner-sharing octahedral tilt angles are 45°. The Mo(3)-O(13) bond length is 2.08 Å. The Mo(3)-O(19) bond length is 2.11 Å. The Mo(3)-O(20) bond length is 2.24 Å. The Mo(3)-O(21) bond length is 1.94 Å. The Mo(3)-O(25) bond length is 1.97 Å. In the fourth Mo site, Mo(4) is bonded to one O(11), one O(16), one O(23), one O(24), and one O(7) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Co(2)O6 octahedra,  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra,  an edgeedge with one Mo(2)O5 square pyramid, and  an edgeedge with one Mo(6)O5 square pyramid. The corner-sharing octahedral tilt angles are 45°. The Mo(4)-O(11) bond length is 2.31 Å. The Mo(4)-O(16) bond length is 2.10 Å. The Mo(4)-O(23) bond length is 1.95 Å. The Mo(4)-O(24) bond length is 1.98 Å. The Mo(4)-O(7) bond length is 2.05 Å. In the fifth Mo site, Mo(5) is bonded to one O(14), one O(19), one O(20), one O(22), and one O(26) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Co(2)O6 octahedra,  a cornercorner with one P(3)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra,  an edgeedge with one Mo(1)O5 square pyramid, and  an edgeedge with one Mo(3)O5 square pyramid. The corner-sharing octahedral tilt angles are 46°. The Mo(5)-O(14) bond length is 2.08 Å. The Mo(5)-O(19) bond length is 2.12 Å. The Mo(5)-O(20) bond length is 2.23 Å. The Mo(5)-O(22) bond length is 1.95 Å. The Mo(5)-O(26) bond length is 1.98 Å. In the sixth Mo site, Mo(6) is bonded to one O(10), one O(12), one O(23), one O(24), and one O(9) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Co(2)O6 octahedra,  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra,  an edgeedge with one Mo(1)O5 square pyramid, and  an edgeedge with one Mo(4)O5 square pyramid. The corner-sharing octahedral tilt angles are 44°. The Mo(6)-O(10) bond length is 2.04 Å. The Mo(6)-O(12) bond length is 2.29 Å. The Mo(6)-O(23) bond length is 1.95 Å. The Mo(6)-O(24) bond length is 1.98 Å. The Mo(6)-O(9) bond length is 2.10 Å. There are two inequivalent Co sites. In the first Co site, Co(1) is bonded to one O(18), one O(5), one O(8), and two equivalent O(17) atoms to form CoO5 square pyramids that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, and  an edgeedge with one Co(1)O5 square pyramid. The Co(1)-O(18) bond length is 2.05 Å. The Co(1)-O(5) bond length is 2.03 Å. The Co(1)-O(8) bond length is 2.05 Å. There is one shorter (2.20 Å) and one longer (2.21 Å) Co(1)-O(17) bond length. In the second Co site, Co(2) is bonded to two equivalent O(24), two equivalent O(25), and two equivalent O(26) atoms to form CoO6 octahedra that share corners with two equivalent Mo(1)O5 square pyramids, corners with two equivalent Mo(2)O5 square pyramids, corners with two equivalent Mo(3)O5 square pyramids, corners with two equivalent Mo(4)O5 square pyramids, corners with two equivalent Mo(5)O5 square pyramids, and corners with two equivalent Mo(6)O5 square pyramids. Both Co(2)-O(24) bond lengths are 2.12 Å. Both Co(2)-O(25) bond lengths are 2.17 Å. Both Co(2)-O(26) bond lengths are 2.15 Å. There are four inequivalent P sites. In the first P site, P(1) is bonded to one O(15), one O(3), one O(5), and one O(7) atom to form PO4 tetrahedra that share  a cornercorner with one Mo(2)O5 square pyramid,  a cornercorner with one Mo(4)O5 square pyramid, and  a cornercorner with one Co(1)O5 square pyramid. The P(1)-O(15) bond length is 1.55 Å. The P(1)-O(3) bond length is 1.53 Å. The P(1)-O(5) bond length is 1.51 Å. The P(1)-O(7) bond length is 1.54 Å. In the second P site, P(2) is bonded to one O(10), one O(2), one O(6), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one Mo(1)O5 square pyramid,  a cornercorner with one Mo(6)O5 square pyramid, and  a cornercorner with one Co(1)O5 square pyramid. The P(2)-O(10) bond length is 1.55 Å. The P(2)-O(2) bond length is 1.52 Å. The P(2)-O(6) bond length is 1.56 Å. The P(2)-O(8) bond length is 1.52 Å. In the third P site, P(3) is bonded to one O(1), one O(13), one O(14), and one O(18) atom to form PO4 tetrahedra that share  a cornercorner with one Mo(3)O5 square pyramid,  a cornercorner with one Mo(5)O5 square pyramid, and  a cornercorner with one Co(1)O5 square pyramid. The P(3)-O(1) bond length is 1.58 Å. The P(3)-O(13) bond length is 1.54 Å. The P(3)-O(14) bond length is 1.53 Å. The P(3)-O(18) bond length is 1.49 Å. In the fourth P site, P(4) is bonded to one O(11), one O(12), one O(20), and one O(4) atom to form PO4 tetrahedra that share  a cornercorner with one Mo(1)O5 square pyramid,  a cornercorner with one Mo(2)O5 square pyramid,  a cornercorner with one Mo(3)O5 square pyramid,  a cornercorner with one Mo(4)O5 square pyramid,  a cornercorner with one Mo(5)O5 square pyramid, and  a cornercorner with one Mo(6)O5 square pyramid. The P(4)-O(11) bond length is 1.55 Å. The P(4)-O(12) bond length is 1.55 Å. The P(4)-O(20) bond length is 1.57 Å. The P(4)-O(4) bond length is 1.49 Å. There are twenty-six inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to one P(3) atom. In the second O site, O(2) is bonded in a single-bond geometry to one P(2) atom. In the third O site, O(3) is bonded in a single-bond geometry to one P(1) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one P(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Co(1) and one P(1) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Mo(1) and one P(2) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one Mo(4) and one P(1) atom. In the eighth O site, O(8) is bonded in a distorted bent 120 degrees geometry to one Co(1) and one P(2) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Mo(1) and one Mo(6) atom. In the tenth O site, O(10) is bonded in a distorted single-bond geometry to one Mo(6) and one P(2) atom. In the eleventh O site, O(11) is bonded in a distorted single-bond geometry to one Mo(2), one Mo(4), and one P(4) atom. In the twelfth O site, O(12) is bonded in a distorted single-bond geometry to one Mo(1), one Mo(6), and one P(4) atom. In the thirteenth O site, O(13) is bonded in a distorted single-bond geometry to one Mo(3) and one P(3) atom. In the fourteenth O site, O(14) is bonded in a distorted single-bond geometry to one Mo(5) and one P(3) atom. In the fifteenth O site, O(15) is bonded in a distorted single-bond geometry to one Mo(2) and one P(1) atom. In the sixteenth O site, O(16) is bonded in a bent 120 degrees geometry to one Mo(2) and one Mo(4) atom. In the seventeenth O site, O(17) is bonded in a water-like geometry to two equivalent Co(1) atoms. In the eighteenth O site, O(18) is bonded in a bent 150 degrees geometry to one Co(1) and one P(3) atom. In the nineteenth O site, O(19) is bonded in a water-like geometry to one Mo(3) and one Mo(5) atom. In the twentieth O site, O(20) is bonded in a distorted single-bond geometry to one Mo(3), one Mo(5), and one P(4) atom. In the twenty-first O site, O(21) is bonded in an L-shaped geometry to one Mo(2) and one Mo(3) atom. In the twenty-second O site, O(22) is bonded in an L-shaped geometry to one Mo(1) and one Mo(5) atom. In the twenty-third O site, O(23) is bonded in an L-shaped geometry to one Mo(4) and one Mo(6) atom. In the twenty-fourth O site, O(24) is bonded in a 3-coordinate geometry to one Mo(4), one Mo(6), and one Co(2) atom. In the twenty-fifth O site, O(25) is bonded in a 3-coordinate geometry to one Mo(2), one Mo(3), and one Co(2) atom. In the twenty-sixth O site, O(26) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(5), and one Co(2) atom. Linkers: 8 [O]P([O])([O])=O. Metal clusters: 3 [Co] ,12 [Mo]. The MOF has largest included sphere 6.23 A, density 1.92 g/cm3, surface area 1880.20 m2/g, accessible volume 0.28 cm3/g