Ga2P3H4(O3F)3 crystallizes in the triclinic P-1 space group. There are three inequivalent Ga sites. In the first Ga site, Ga(1) is bonded to one O(1), one O(2), one O(3), one O(4), one F(2), and one F(3) atom to form GaO4F2 octahedra that share  a cornercorner with one P(1)HO3 tetrahedra,  a cornercorner with one P(2)HO3 tetrahedra, and corners with two equivalent P(3)HO3 tetrahedra. The Ga(1)-O(1) bond length is 1.96 Å. The Ga(1)-O(2) bond length is 1.96 Å. The Ga(1)-O(3) bond length is 1.99 Å. The Ga(1)-O(4) bond length is 1.97 Å. The Ga(1)-F(2) bond length is 1.89 Å. The Ga(1)-F(3) bond length is 1.89 Å. In the second Ga site, Ga(2) is bonded to two equivalent O(5), two equivalent O(8), and two equivalent F(1) atoms to form GaO4F2 octahedra that share corners with two equivalent Ga(3)O4F2 octahedra, corners with two equivalent P(1)HO3 tetrahedra, and corners with two equivalent P(2)HO3 tetrahedra. The corner-sharing octahedral tilt angles are 50°. Both Ga(2)-O(5) bond lengths are 1.94 Å. Both Ga(2)-O(8) bond lengths are 1.96 Å. Both Ga(2)-F(1) bond lengths are 1.95 Å. In the third Ga site, Ga(3) is bonded to two equivalent O(6), two equivalent O(7), and two equivalent F(1) atoms to form GaO4F2 octahedra that share corners with two equivalent Ga(2)O4F2 octahedra, corners with two equivalent P(1)HO3 tetrahedra, and corners with two equivalent P(2)HO3 tetrahedra. The corner-sharing octahedral tilt angles are 50°. Both Ga(3)-O(6) bond lengths are 1.94 Å. Both Ga(3)-O(7) bond lengths are 1.94 Å. Both Ga(3)-F(1) bond lengths are 1.97 Å. There are three inequivalent P sites. In the first P site, P(1) is bonded to one H(3), one O(4), one O(5), and one O(7) atom to form distorted PHO3 tetrahedra that share  a cornercorner with one Ga(1)O4F2 octahedra,  a cornercorner with one Ga(2)O4F2 octahedra, and  a cornercorner with one Ga(3)O4F2 octahedra. The corner-sharing octahedral tilt angles range from 39-48°. The P(1)-H(3) bond length is 1.39 Å. The P(1)-O(4) bond length is 1.53 Å. The P(1)-O(5) bond length is 1.52 Å. The P(1)-O(7) bond length is 1.52 Å. In the second P site, P(2) is bonded to one H(2), one O(2), one O(6), and one O(8) atom to form PHO3 tetrahedra that share  a cornercorner with one Ga(1)O4F2 octahedra,  a cornercorner with one Ga(2)O4F2 octahedra, and  a cornercorner with one Ga(3)O4F2 octahedra. The corner-sharing octahedral tilt angles range from 40-49°. The P(2)-H(2) bond length is 1.29 Å. The P(2)-O(2) bond length is 1.52 Å. The P(2)-O(6) bond length is 1.52 Å. The P(2)-O(8) bond length is 1.53 Å. In the third P site, P(3) is bonded to one H(1), one O(1), one O(3), and one O(9) atom to form distorted PHO3 tetrahedra that share corners with two equivalent Ga(1)O4F2 octahedra. The corner-sharing octahedral tilt angles range from 47-55°. The P(3)-H(1) bond length is 1.35 Å. The P(3)-O(1) bond length is 1.52 Å. The P(3)-O(3) bond length is 1.51 Å. The P(3)-O(9) bond length is 1.56 Å. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one P(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one P(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one P(1) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(9) atom. The H(4)-O(9) bond length is 0.85 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ga(1) and one P(3) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Ga(1) and one P(2) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ga(1) and one P(3) atom. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one Ga(1) and one P(1) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Ga(2) and one P(1) atom. In the sixth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Ga(3) and one P(2) atom. In the seventh O site, O(7) is bonded in a distorted bent 150 degrees geometry to one Ga(3) and one P(1) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Ga(2) and one P(2) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one P(3) and one H(4) atom. There are three inequivalent F sites. In the first F site, F(1) is bonded in a bent 120 degrees geometry to one Ga(2) and one Ga(3) atom. In the second F site, F(2) is bonded in a single-bond geometry to one Ga(1) atom. In the third F site, F(3) is bonded in a single-bond geometry to one Ga(1) atom. Linkers: 2 [O][PH](=O)O ,4 [O][PH]([O])=O. Metal clusters: 4 [Ga]. The MOF has largest included sphere 4.38 A, density 2.08 g/cm3, surface area 2691.41 m2/g, accessible volume 0.19 cm3/g