Cu2C24SO3CF3 crystallizes in the monoclinic C2 space group. The structure consists of four trifluoromethane molecules inside a Cu2C24SO3 framework. In the Cu2C24SO3 framework, there are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a rectangular see-saw-like geometry to one C(3), one C(4), one C(7), and one C(8) atom. The Cu(1)-C(3) bond length is 2.09 Å. The Cu(1)-C(4) bond length is 2.14 Å. The Cu(1)-C(7) bond length is 2.09 Å. The Cu(1)-C(8) bond length is 2.11 Å. In the second Cu site, Cu(2) is bonded in a 6-coordinate geometry to one C(13), one C(14), one C(19), one C(20), one O(1), and one O(3) atom. The Cu(2)-C(13) bond length is 2.07 Å. The Cu(2)-C(14) bond length is 2.14 Å. The Cu(2)-C(19) bond length is 2.13 Å. The Cu(2)-C(20) bond length is 2.13 Å. The Cu(2)-O(1) bond length is 2.27 Å. The Cu(2)-O(3) bond length is 2.15 Å. There are twenty-four inequivalent C sites. In the first C site, C(1) is bonded in a water-like geometry to one C(2) and one C(6) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-C(6) bond length is 1.51 Å. In the second C site, C(2) is bonded in a water-like geometry to one C(1) and one C(3) atom. The C(2)-C(3) bond length is 1.51 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(2), and one C(4) atom. The C(3)-C(4) bond length is 1.20 Å. In the fourth C site, C(4) is bonded in a 3-coordinate geometry to one Cu(1), one C(3), and one C(5) atom. The C(4)-C(5) bond length is 1.47 Å. In the fifth C site, C(5) is bonded in a water-like geometry to one C(4) and one C(6) atom. The C(5)-C(6) bond length is 1.56 Å. In the sixth C site, C(6) is bonded in a bent 120 degrees geometry to one C(1) and one C(5) atom. In the seventh C site, C(7) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(18), and one C(8) atom. The C(7)-C(18) bond length is 1.52 Å. The C(7)-C(8) bond length is 1.17 Å. In the eighth C site, C(8) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(7), and one C(9) atom. The C(8)-C(9) bond length is 1.48 Å. In the ninth C site, C(9) is bonded in a bent 120 degrees geometry to one C(10) and one C(8) atom. The C(9)-C(10) bond length is 1.53 Å. In the tenth C site, C(10) is bonded in a water-like geometry to one C(11) and one C(9) atom. The C(10)-C(11) bond length is 1.51 Å. In the eleventh C site, C(11) is bonded in a bent 120 degrees geometry to one C(10) and one C(12) atom. The C(11)-C(12) bond length is 1.55 Å. In the twelfth C site, C(12) is bonded in a water-like geometry to one C(11) and one C(13) atom. The C(12)-C(13) bond length is 1.49 Å. In the thirteenth C site, C(13) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(12), and one C(14) atom. The C(13)-C(14) bond length is 1.21 Å. In the fourteenth C site, C(14) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(13), and one C(15) atom. The C(14)-C(15) bond length is 1.44 Å. In the fifteenth C site, C(15) is bonded in a water-like geometry to one C(14) and one C(16) atom. The C(15)-C(16) bond length is 1.51 Å. In the sixteenth C site, C(16) is bonded in a bent 120 degrees geometry to one C(15) and one C(17) atom. The C(16)-C(17) bond length is 1.51 Å. In the seventeenth C site, C(17) is bonded in a bent 120 degrees geometry to one C(16) and one C(18) atom. The C(17)-C(18) bond length is 1.53 Å. In the eighteenth C site, C(18) is bonded in a water-like geometry to one C(17) and one C(7) atom. In the nineteenth C site, C(19) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(20), and one C(24) atom. The C(19)-C(20) bond length is 1.18 Å. The C(19)-C(24) bond length is 1.49 Å. In the twentieth C site, C(20) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(19), and one C(21) atom. The C(20)-C(21) bond length is 1.50 Å. In the twenty-first C site, C(21) is bonded in a bent 120 degrees geometry to one C(20) and one C(22) atom. The C(21)-C(22) bond length is 1.53 Å. In the twenty-second C site, C(22) is bonded in a bent 120 degrees geometry to one C(21) and one C(23) atom. The C(22)-C(23) bond length is 1.51 Å. In the twenty-third C site, C(23) is bonded in a bent 120 degrees geometry to one C(22) and one C(24) atom. The C(23)-C(24) bond length is 1.54 Å. In the twenty-fourth C site, C(24) is bonded in a water-like geometry to one C(19) and one C(23) atom. S(1) is bonded in a distorted trigonal non-coplanar geometry to one O(1), one O(2), and one O(3) atom. The S(1)-O(1) bond length is 1.45 Å. The S(1)-O(2) bond length is 1.44 Å. The S(1)-O(3) bond length is 1.46 Å. There are three inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to one Cu(2) and one S(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one S(1) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Cu(2) and one S(1) atom. Linkers: 3 [C]1[C][C][C]([Cu][C]2[C][C][C][C][C]C#C[C][C][C][C]2)[C][C][C][C][C][C]([Cu][C]2[C][C][C][C][C]C#C[C][C][C][C]2)[C][C]1 ,2 [C][C][C][C][C]([C])[Cu][C]1[C][C][C][C][C][C]([Cu][C]2[C][C][C][C][C]C#C[C][C][C][C]2)[C][C][C][C][C]1 ,2 [C]1[C][C]C#C[C][C][C][C]C#C[C]1. Metal clusters: 4 [Cu]. The MOF has largest included sphere 5.07 A, density 1.23 g/cm3, surface area 4929.53 m2/g, accessible volume 0.29 cm3/g