In9H36(C54O25)2 crystallizes in the trigonal R32 space group. There are two inequivalent In sites. In the first In site, In(1) is bonded to one O(1), one O(2), one O(3), one O(4), and one O(9) atom to form corner-sharing InO5 square pyramids. The In(1)-O(1) bond length is 2.19 Å. The In(1)-O(2) bond length is 2.18 Å. The In(1)-O(3) bond length is 2.15 Å. The In(1)-O(4) bond length is 2.15 Å. The In(1)-O(9) bond length is 2.03 Å. In the second In site, In(2) is bonded in a distorted hexagonal bipyramidal geometry to two equivalent O(5), two equivalent O(6), two equivalent O(7), and two equivalent O(8) atoms. Both In(2)-O(5) bond lengths are 2.27 Å. Both In(2)-O(6) bond lengths are 2.33 Å. Both In(2)-O(7) bond lengths are 2.28 Å. Both In(2)-O(8) bond lengths are 2.26 Å. There are eighteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(2), and one O(3) atom. The C(1)-C(6) bond length is 1.49 Å. The C(1)-O(2) bond length is 1.21 Å. The C(1)-O(3) bond length is 1.30 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(3), one C(4), and one H(1) atom. The C(2)-C(3) bond length is 1.41 Å. The C(2)-C(4) bond length is 1.41 Å. The C(2)-H(1) bond length is 0.93 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(11), one C(2), and one C(7) atom. The C(3)-C(11) bond length is 1.48 Å. The C(3)-C(7) bond length is 1.40 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(18), one C(2), and one C(5) atom. The C(4)-C(18) bond length is 1.47 Å. The C(4)-C(5) bond length is 1.42 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(4), one C(6), and one H(2) atom. The C(5)-C(6) bond length is 1.41 Å. The C(5)-H(2) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(1), one C(5), and one C(7) atom. The C(6)-C(7) bond length is 1.38 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(3), one C(6), and one H(3) atom. The C(7)-H(3) bond length is 0.93 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(10), one C(14), and one C(9) atom. The C(8)-C(10) bond length is 1.36 Å. The C(8)-C(14) bond length is 1.40 Å. The C(8)-C(9) bond length is 1.50 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(1), and one O(4) atom. The C(9)-O(1) bond length is 1.17 Å. The C(9)-O(4) bond length is 1.29 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(13), one C(8), and one H(4) atom. The C(10)-C(13) bond length is 1.40 Å. The C(10)-H(4) bond length is 0.93 Å. In the eleventh C site, C(11) is bonded in a linear geometry to one C(12) and one C(3) atom. The C(11)-C(12) bond length is 1.16 Å. In the twelfth C site, C(12) is bonded in a linear geometry to one C(11) and one C(13) atom. The C(12)-C(13) bond length is 1.43 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(16) atom. The C(13)-C(16) bond length is 1.42 Å. In the fourteenth C site, C(14) is bonded in a distorted single-bond geometry to one C(15), one C(8), and one H(5) atom. The C(14)-C(15) bond length is 1.41 Å. The C(14)-H(5) bond length is 0.93 Å. In the fifteenth C site, C(15) is bonded in a trigonal planar geometry to one C(14), one C(16), and one C(17) atom. The C(15)-C(16) bond length is 1.40 Å. The C(15)-C(17) bond length is 1.52 Å. In the sixteenth C site, C(16) is bonded in a distorted trigonal planar geometry to one C(13), one C(15), and one H(6) atom. The C(16)-H(6) bond length is 0.93 Å. In the seventeenth C site, C(17) is bonded in a bent 120 degrees geometry to one C(15), one O(5), and one O(6) atom. The C(17)-O(5) bond length is 1.25 Å. The C(17)-O(6) bond length is 1.29 Å. In the eighteenth C site, C(18) is bonded in a bent 120 degrees geometry to one C(4), one O(7), and one O(8) atom. The C(18)-O(7) bond length is 1.29 Å. The C(18)-O(8) bond length is 1.23 Å. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(10) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(14) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(16) atom. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a 2-coordinate geometry to one In(1) and one C(9) atom. In the second O site, O(2) is bonded in a 2-coordinate geometry to one In(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one In(1) and one C(1) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one In(1) and one C(9) atom. In the fifth O site, O(5) is bonded in an L-shaped geometry to one In(2) and one C(17) atom. In the sixth O site, O(6) is bonded in an L-shaped geometry to one In(2) and one C(17) atom. In the seventh O site, O(7) is bonded in an L-shaped geometry to one In(2) and one C(18) atom. In the eighth O site, O(8) is bonded in an L-shaped geometry to one In(2) and one C(18) atom. In the ninth O site, O(9) is bonded in a trigonal planar geometry to three equivalent In(1) atoms. Linkers: 18 [O]C(=O)c1cc(C#Cc2cc(C([O])=O)cc(C([O])=O)c2)cc(C([O])=O)c1. Metal clusters: 6 O=[C]O[In](O[C]=O)O[In](O[C]=O)O[C]=O.O=[C]O[In]O[C]=O ,9 [O][C]=O.[O][C]O[In](O[C][O])O[C][O]. The MOF has largest included sphere 12.19 A, density 0.88 g/cm3, surface area 3401.73 m2/g, accessible volume 0.73 cm3/g