Ga3P3HO13F3 crystallizes in the monoclinic C2/c space group. There are three inequivalent Ga sites. In the first Ga site, Ga(1) is bonded to one O(2), one O(3), one O(5), one O(6), and two equivalent F(1) atoms to form GaO4F2 octahedra that share  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, corners with two equivalent P(1)O4 tetrahedra, and  an edgeedge with one Ga(1)O4F2 octahedra. The Ga(1)-O(2) bond length is 1.92 Å. The Ga(1)-O(3) bond length is 1.94 Å. The Ga(1)-O(5) bond length is 1.89 Å. The Ga(1)-O(6) bond length is 1.92 Å. There is one shorter (1.99 Å) and one longer (2.00 Å) Ga(1)-F(1) bond length. In the second Ga site, Ga(2) is bonded in a 7-coordinate geometry to one H(1), one O(1), one O(10), one O(11), one O(13), one F(2), and one F(3) atom. The Ga(2)-H(1) bond length is 1.67 Å. The Ga(2)-O(1) bond length is 1.90 Å. The Ga(2)-O(10) bond length is 1.92 Å. The Ga(2)-O(11) bond length is 1.90 Å. The Ga(2)-O(13) bond length is 1.92 Å. The Ga(2)-F(2) bond length is 2.03 Å. The Ga(2)-F(3) bond length is 1.98 Å. In the third Ga site, Ga(3) is bonded to one O(13), one O(4), one O(7), one O(8), one F(2), and one F(3) atom to form GaO4F2 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(2)O4 tetrahedra, and  a cornercorner with one P(3)O4 tetrahedra. The Ga(3)-O(13) bond length is 1.90 Å. The Ga(3)-O(4) bond length is 1.98 Å. The Ga(3)-O(7) bond length is 1.90 Å. The Ga(3)-O(8) bond length is 1.96 Å. The Ga(3)-F(2) bond length is 1.94 Å. The Ga(3)-F(3) bond length is 1.98 Å. There are three inequivalent P sites. In the first P site, P(1) is bonded to one O(1), one O(2), one O(3), and one O(4) atom to form PO4 tetrahedra that share  a cornercorner with one Ga(3)O4F2 octahedra and corners with two equivalent Ga(1)O4F2 octahedra. The corner-sharing octahedral tilt angles range from 48-55°. The P(1)-O(1) bond length is 1.53 Å. The P(1)-O(2) bond length is 1.53 Å. The P(1)-O(3) bond length is 1.55 Å. The P(1)-O(4) bond length is 1.55 Å. In the second P site, P(2) is bonded to one O(10), one O(6), one O(8), and one O(9) atom to form PO4 tetrahedra that share  a cornercorner with one Ga(1)O4F2 octahedra and  a cornercorner with one Ga(3)O4F2 octahedra. The corner-sharing octahedral tilt angles are 43°. The P(2)-O(10) bond length is 1.53 Å. The P(2)-O(6) bond length is 1.52 Å. The P(2)-O(8) bond length is 1.51 Å. The P(2)-O(9) bond length is 1.60 Å. In the third P site, P(3) is bonded to one O(11), one O(12), one O(5), and one O(7) atom to form PO4 tetrahedra that share  a cornercorner with one Ga(1)O4F2 octahedra and  a cornercorner with one Ga(3)O4F2 octahedra. The corner-sharing octahedral tilt angles range from 37-52°. The P(3)-O(11) bond length is 1.55 Å. The P(3)-O(12) bond length is 1.57 Å. The P(3)-O(5) bond length is 1.50 Å. The P(3)-O(7) bond length is 1.55 Å. H(1) is bonded in a single-bond geometry to one Ga(2) and one O(13) atom. The H(1)-O(13) bond length is 0.86 Å. There are thirteen inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ga(2) and one P(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ga(1) and one P(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ga(1) and one P(1) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ga(3) and one P(1) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Ga(1) and one P(3) atom. In the sixth O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Ga(1) and one P(2) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Ga(3) and one P(3) atom. In the eighth O site, O(8) is bonded in a distorted bent 150 degrees geometry to one Ga(3) and one P(2) atom. In the ninth O site, O(9) is bonded in a single-bond geometry to one P(2) atom. In the tenth O site, O(10) is bonded in a distorted bent 120 degrees geometry to one Ga(2) and one P(2) atom. In the eleventh O site, O(11) is bonded in a bent 120 degrees geometry to one Ga(2) and one P(3) atom. In the twelfth O site, O(12) is bonded in a single-bond geometry to one P(3) atom. In the thirteenth O site, O(13) is bonded in a distorted single-bond geometry to one Ga(2), one Ga(3), and one H(1) atom. There are three inequivalent F sites. In the first F site, F(1) is bonded in a water-like geometry to two equivalent Ga(1) atoms. In the second F site, F(2) is bonded in a water-like geometry to one Ga(2) and one Ga(3) atom. In the third F site, F(3) is bonded in a water-like geometry to one Ga(2) and one Ga(3) atom. Linkers: 24 [O]P([O])([O])=O ,8 [OH]. Metal clusters: 24 [Ga]. The MOF has largest included sphere 4.82 A, density 2.23 g/cm3, surface area 2240.20 m2/g, accessible volume 0.18 cm3/g