GaC24N2O5 crystallizes in the orthorhombic Cmmm space group. Ga(1) is bonded to two equivalent O(2) and four equivalent O(1) atoms to form corner-sharing GaO6 octahedra. The corner-sharing octahedral tilt angles are 50°. Both Ga(1)-O(2) bond lengths are 1.85 Å. All Ga(1)-O(1) bond lengths are 2.00 Å. There are ten inequivalent C sites. In the first C site, C(1) is bonded in a bent 120 degrees geometry to one C(2) and one C(8) atom. The C(1)-C(2) bond length is 1.41 Å. The C(1)-C(8) bond length is 1.43 Å. In the second C site, C(2) is bonded in a bent 120 degrees geometry to one C(1) and one C(9) atom. The C(2)-C(9) bond length is 1.40 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(4), one C(7), and one N(1) atom. The C(3)-C(4) bond length is 1.43 Å. The C(3)-C(7) bond length is 1.35 Å. The C(3)-N(1) bond length is 1.36 Å. In the fourth C site, C(4) is bonded in a single-bond geometry to one C(3) atom. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(6), one C(7), and one N(2) atom. The C(5)-C(6) bond length is 1.33 Å. The C(5)-C(7) bond length is 1.37 Å. The C(5)-N(2) bond length is 1.36 Å. In the sixth C site, C(6) is bonded in a single-bond geometry to one C(5) atom. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(8) atom. The C(7)-C(8) bond length is 1.51 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(7) and two equivalent C(1) atoms. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(10) and two equivalent C(2) atoms. The C(9)-C(10) bond length is 1.57 Å. In the tenth C site, C(10) is bonded in a bent 150 degrees geometry to one C(9) and two equivalent O(1) atoms. Both C(10)-O(1) bond lengths are 1.30 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a water-like geometry to two equivalent C(3) atoms. In the second N site, N(2) is bonded in a water-like geometry to two equivalent C(5) atoms. There are two inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ga(1) and one C(10) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to two equivalent Ga(1) atoms. Linkers: 2 [O]C(=O)c1[c][c]c(/C2=C3\[C]=[C]/C(=C(\c4[c][c]c(C([O])=O)[c][c]4)C4=N/C(=C(/c5[c][c]c(C([O])=O)[c][c]5)C5=[C][C]=C([N]5)/C(c5[c][c]c(C([O])=O)[c][c]5)=C5/[C]=[C]C2=N5)[C]=[C]4)[N]3)[c][c]1. Metal clusters: 4 [Ga]. RCSR code: scu. The MOF has largest included sphere 7.25 A, density 0.85 g/cm3, surface area 4009.28 m2/g, accessible volume 0.73 cm3/g