Mo12Fe3P8(HO26)2 crystallizes in the monoclinic P2_1/c space group. There are six inequivalent Mo sites. In the first Mo site, Mo(1) is bonded to one O(14), one O(15), one O(2), one O(4), and one O(8) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Fe(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(3)O5 square pyramid. The corner-sharing octahedral tilt angles are 46°. The Mo(1)-O(14) bond length is 2.29 Å. The Mo(1)-O(15) bond length is 2.11 Å. The Mo(1)-O(2) bond length is 1.94 Å. The Mo(1)-O(4) bond length is 1.98 Å. The Mo(1)-O(8) bond length is 2.03 Å. In the second Mo site, Mo(2) is bonded to one O(12), one O(14), one O(15), one O(3), and one O(5) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Fe(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(6)O5 square pyramid. The corner-sharing octahedral tilt angles are 46°. The Mo(2)-O(12) bond length is 2.08 Å. The Mo(2)-O(14) bond length is 2.23 Å. The Mo(2)-O(15) bond length is 2.13 Å. The Mo(2)-O(3) bond length is 1.97 Å. The Mo(2)-O(5) bond length is 1.93 Å. In the third Mo site, Mo(3) is bonded to one O(11), one O(2), one O(23), one O(4), and one O(9) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)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 46°. The Mo(3)-O(11) bond length is 2.27 Å. The Mo(3)-O(2) bond length is 1.93 Å. The Mo(3)-O(23) bond length is 2.06 Å. The Mo(3)-O(4) bond length is 1.97 Å. The Mo(3)-O(9) bond length is 2.11 Å. In the fourth Mo site, Mo(4) is bonded to one O(11), one O(16), one O(22), one O(7), and one O(9) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra,  an edgeedge with one Mo(3)O5 square pyramid, and  an edgeedge with one Mo(5)O5 square pyramid. The corner-sharing octahedral tilt angles are 45°. The Mo(4)-O(11) bond length is 2.28 Å. The Mo(4)-O(16) bond length is 1.94 Å. The Mo(4)-O(22) bond length is 2.07 Å. The Mo(4)-O(7) bond length is 1.97 Å. The Mo(4)-O(9) bond length is 2.12 Å. In the fifth Mo site, Mo(5) is bonded to one O(13), one O(16), one O(19), one O(6), and one O(7) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra,  an edgeedge with one Mo(4)O5 square pyramid, and  an edgeedge with one Mo(6)O5 square pyramid. The corner-sharing octahedral tilt angles are 46°. The Mo(5)-O(13) bond length is 2.30 Å. The Mo(5)-O(16) bond length is 1.94 Å. The Mo(5)-O(19) bond length is 2.12 Å. The Mo(5)-O(6) bond length is 2.03 Å. The Mo(5)-O(7) bond length is 1.99 Å. In the sixth Mo site, Mo(6) is bonded to one O(13), one O(18), one O(19), one O(3), and one O(5) atom to form distorted MoO5 square pyramids that share  a cornercorner with one Fe(2)O6 octahedra,  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(3)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 47°. The Mo(6)-O(13) bond length is 2.30 Å. The Mo(6)-O(18) bond length is 2.04 Å. The Mo(6)-O(19) bond length is 2.09 Å. The Mo(6)-O(3) bond length is 1.98 Å. The Mo(6)-O(5) bond length is 1.95 Å. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded to one O(1), one O(10), one O(20), one O(21), one O(25), and one O(26) atom to form FeO6 octahedra 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 corners with two equivalent P(4)O4 tetrahedra. The Fe(1)-O(1) bond length is 2.18 Å. The Fe(1)-O(10) bond length is 2.32 Å. The Fe(1)-O(20) bond length is 2.15 Å. The Fe(1)-O(21) bond length is 2.07 Å. The Fe(1)-O(25) bond length is 2.13 Å. The Fe(1)-O(26) bond length is 2.23 Å. In the second Fe site, Fe(2) is bonded to two equivalent O(3), two equivalent O(4), and two equivalent O(7) atoms to form FeO6 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 Fe(2)-O(3) bond lengths are 2.21 Å. Both Fe(2)-O(4) bond lengths are 2.16 Å. Both Fe(2)-O(7) bond lengths are 2.20 Å. There are four inequivalent P sites. In the first P site, P(1) is bonded to one O(17), one O(18), one O(20), and one O(6) atom to form PO4 tetrahedra that share  a cornercorner with one Fe(1)O6 octahedra,  a cornercorner with one Mo(5)O5 square pyramid, and  a cornercorner with one Mo(6)O5 square pyramid. The corner-sharing octahedral tilt angles are 52°. The P(1)-O(17) bond length is 1.54 Å. The P(1)-O(18) bond length is 1.55 Å. The P(1)-O(20) bond length is 1.51 Å. The P(1)-O(6) bond length is 1.55 Å. In the second P site, P(2) is bonded to one O(22), one O(23), one O(24), and one O(25) atom to form PO4 tetrahedra that share  a cornercorner with one Fe(1)O6 octahedra,  a cornercorner with one Mo(3)O5 square pyramid, and  a cornercorner with one Mo(4)O5 square pyramid. The corner-sharing octahedral tilt angles are 39°. The P(2)-O(22) bond length is 1.53 Å. The P(2)-O(23) bond length is 1.55 Å. The P(2)-O(24) bond length is 1.58 Å. The P(2)-O(25) bond length is 1.49 Å. In the third P site, P(3) is bonded to one O(1), one O(11), one O(13), and one O(14) atom to form PO4 tetrahedra that share  a cornercorner with one Fe(1)O6 octahedra,  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 corner-sharing octahedral tilt angles are 46°. The P(3)-O(1) bond length is 1.51 Å. The P(3)-O(11) bond length is 1.56 Å. The P(3)-O(13) bond length is 1.54 Å. The P(3)-O(14) bond length is 1.56 Å. In the fourth P site, P(4) is bonded to one O(10), one O(12), one O(21), and one O(8) atom to form PO4 tetrahedra that share corners with two equivalent Fe(1)O6 octahedra,  a cornercorner with one Mo(1)O5 square pyramid, and  a cornercorner with one Mo(2)O5 square pyramid. The corner-sharing octahedral tilt angles are 34°. The P(4)-O(10) bond length is 1.57 Å. The P(4)-O(12) bond length is 1.55 Å. The P(4)-O(21) bond length is 1.49 Å. The P(4)-O(8) bond length is 1.54 Å. H(1) is bonded in a single-bond geometry to one O(26) atom. The H(1)-O(26) bond length is 0.82 Å. There are twenty-six inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Fe(1) and one P(3) atom. In the second O site, O(2) is bonded in an L-shaped geometry to one Mo(1) and one Mo(3) atom. In the third O site, O(3) is bonded in a 3-coordinate geometry to one Mo(2), one Mo(6), and one Fe(2) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(3), and one Fe(2) atom. In the fifth O site, O(5) is bonded in an L-shaped geometry to one Mo(2) and one Mo(6) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Mo(5) and one P(1) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to one Mo(4), one Mo(5), and one Fe(2) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one Mo(1) and one P(4) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Mo(3) and one Mo(4) atom. In the tenth O site, O(10) is bonded in a bent 150 degrees geometry to one Fe(1) and one P(4) atom. In the eleventh O site, O(11) is bonded in a distorted single-bond geometry to one Mo(3), one Mo(4), and one P(3) atom. In the twelfth O site, O(12) is bonded in a distorted single-bond geometry to one Mo(2) and one P(4) atom. In the thirteenth O site, O(13) is bonded in a distorted single-bond geometry to one Mo(5), one Mo(6), and one P(3) atom. In the fourteenth O site, O(14) is bonded in a distorted single-bond geometry to one Mo(1), one Mo(2), and one P(3) atom. In the fifteenth O site, O(15) is bonded in a water-like geometry to one Mo(1) and one Mo(2) atom. In the sixteenth O site, O(16) is bonded in an L-shaped geometry to one Mo(4) and one Mo(5) atom. In the seventeenth O site, O(17) is bonded in a single-bond geometry to one P(1) atom. In the eighteenth O site, O(18) is bonded in a distorted bent 120 degrees geometry to one Mo(6) and one P(1) atom. In the nineteenth O site, O(19) is bonded in a bent 120 degrees geometry to one Mo(5) and one Mo(6) atom. In the twentieth O site, O(20) is bonded in a bent 120 degrees geometry to one Fe(1) and one P(1) atom. In the twenty-first O site, O(21) is bonded in a bent 150 degrees geometry to one Fe(1) and one P(4) atom. In the twenty-second O site, O(22) is bonded in a distorted single-bond geometry to one Mo(4) and one P(2) atom. In the twenty-third O site, O(23) is bonded in a distorted single-bond geometry to one Mo(3) and one P(2) atom. In the twenty-fourth O site, O(24) is bonded in a single-bond geometry to one P(2) atom. In the twenty-fifth O site, O(25) is bonded in a distorted bent 150 degrees geometry to one Fe(1) and one P(2) atom. In the twenty-sixth O site, O(26) is bonded in a water-like geometry to one Fe(1) and one H(1) atom. Linkers: 16 [O]P([O])([O])=O. Metal clusters: 6 [Fe] ,24 [Mo]. The MOF has largest included sphere 5.56 A, density 2.38 g/cm3, surface area 1742.66 m2/g, accessible volume 0.17 cm3/g