Ni4C9H11(SO4)4CH(CH3)2 crystallizes in the trigonal R-3 space group. The structure consists of eighteen 02329_fluka molecules and thirty-six 02329_fluka molecules inside a Ni4C9H11(SO4)4 framework. In the Ni4C9H11(SO4)4 framework, there are four inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(11), one O(15), one O(16), one O(2), one O(5), and one O(9) atom to form NiO6 octahedra that share  a cornercorner with one S(1)O4 tetrahedra,  a cornercorner with one S(2)O4 tetrahedra,  an edgeedge with one Ni(2)O6 octahedra,  an edgeedge with one Ni(3)O5 square pyramid, and  an edgeedge with one Ni(4)O5 square pyramid. The Ni(1)-O(11) bond length is 2.18 Å. The Ni(1)-O(15) bond length is 2.09 Å. The Ni(1)-O(16) bond length is 2.05 Å. The Ni(1)-O(2) bond length is 1.96 Å. The Ni(1)-O(5) bond length is 2.03 Å. The Ni(1)-O(9) bond length is 2.09 Å. In the second Ni site, Ni(2) is bonded to one O(14), one O(15), one O(3), one O(5), one O(6), and one O(7) atom to form NiO6 octahedra that share  a cornercorner with one Ni(4)O5 square pyramid,  a cornercorner with one S(1)O4 tetrahedra,  a cornercorner with one S(2)O4 tetrahedra,  an edgeedge with one Ni(1)O6 octahedra, and  an edgeedge with one Ni(3)O5 square pyramid. The Ni(2)-O(14) bond length is 2.05 Å. The Ni(2)-O(15) bond length is 2.15 Å. The Ni(2)-O(3) bond length is 1.99 Å. The Ni(2)-O(5) bond length is 2.06 Å. The Ni(2)-O(6) bond length is 2.01 Å. The Ni(2)-O(7) bond length is 2.05 Å. In the third Ni site, Ni(3) is bonded to one O(12), one O(16), one O(5), one O(6), and one O(8) atom to form NiO5 square pyramids that share  a cornercorner with one Ni(4)O5 square pyramid,  a cornercorner with one S(1)O4 tetrahedra,  a cornercorner with one S(2)O4 tetrahedra,  an edgeedge with one Ni(1)O6 octahedra, and  an edgeedge with one Ni(2)O6 octahedra. The Ni(3)-O(12) bond length is 2.05 Å. The Ni(3)-O(16) bond length is 2.13 Å. The Ni(3)-O(5) bond length is 2.00 Å. The Ni(3)-O(6) bond length is 2.04 Å. The Ni(3)-O(8) bond length is 2.04 Å. In the fourth Ni site, Ni(4) is bonded to one O(1), one O(11), one O(4), one O(6), and one O(9) atom to form NiO5 square pyramids that share  a cornercorner with one Ni(2)O6 octahedra,  a cornercorner with one Ni(3)O5 square pyramid,  a cornercorner with one S(1)O4 tetrahedra,  a cornercorner with one S(2)O4 tetrahedra, and  an edgeedge with one Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles are 61°. The Ni(4)-O(1) bond length is 2.06 Å. The Ni(4)-O(11) bond length is 2.05 Å. The Ni(4)-O(4) bond length is 1.97 Å. The Ni(4)-O(6) bond length is 2.00 Å. The Ni(4)-O(9) bond length is 2.21 Å. There are nine inequivalent C sites. In the first C site, C(1) is bonded in a bent 120 degrees geometry to one C(3), one O(1), and one O(2) atom. The C(1)-C(3) bond length is 1.41 Å. The C(1)-O(1) bond length is 1.34 Å. The C(1)-O(2) bond length is 1.26 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(3), and one O(4) atom. The C(2)-C(5) bond length is 1.45 Å. The C(2)-O(3) bond length is 1.25 Å. The C(2)-O(4) bond length is 1.29 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.47 Å. The C(3)-C(8) bond length is 1.38 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(1) atom. The C(4)-C(5) bond length is 1.40 Å. The C(4)-H(1) bond length is 0.95 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(6) atom. The C(5)-C(6) bond length is 1.41 Å. In the sixth C site, C(6) is bonded in a single-bond geometry to one C(5) and one H(2) atom. The C(6)-H(2) bond length is 0.95 Å. In the seventh C site, C(8) is bonded in a distorted single-bond geometry to one C(3) and one H(4) atom. The C(8)-H(4) bond length is 0.95 Å. In the eighth C site, C(11) is bonded in a trigonal non-coplanar geometry to one H(13), one H(14), one H(15), and one S(4) atom. The C(11)-H(13) bond length is 0.98 Å. The C(11)-H(14) bond length is 0.98 Å. The C(11)-H(15) bond length is 0.98 Å. The C(11)-S(4) bond length is 1.70 Å. In the ninth C site, C(12) is bonded in a trigonal non-coplanar geometry to one H(16), one H(17), one H(18), and one S(4) atom. The C(12)-H(16) bond length is 0.98 Å. The C(12)-H(17) bond length is 0.98 Å. The C(12)-H(18) bond length is 0.98 Å. The C(12)-S(4) bond length is 1.77 Å. There are eleven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(6) atom. In the third H site, H(4) is bonded in a single-bond geometry to one C(8) atom. In the fourth H site, H(5) is bonded in a single-bond geometry to one O(5) atom. The H(5)-O(5) bond length is 1.00 Å. In the fifth H site, H(6) is bonded in a single-bond geometry to one O(6) atom. The H(6)-O(6) bond length is 1.00 Å. In the sixth H site, H(13) is bonded in a single-bond geometry to one C(11) atom. In the seventh H site, H(14) is bonded in a single-bond geometry to one C(11) atom. In the eighth H site, H(15) is bonded in a single-bond geometry to one C(11) atom. In the ninth H site, H(16) is bonded in a single-bond geometry to one C(12) atom. In the tenth H site, H(17) is bonded in a single-bond geometry to one C(12) atom. In the eleventh H site, H(18) is bonded in a single-bond geometry to one C(12) atom. There are four inequivalent S sites. In the first S site, S(1) is bonded to one O(10), one O(7), one O(8), and one O(9) atom to form SO4 tetrahedra that share  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one Ni(2)O6 octahedra,  a cornercorner with one Ni(3)O5 square pyramid, and  a cornercorner with one Ni(4)O5 square pyramid. The corner-sharing octahedral tilt angles are 56°. The S(1)-O(10) bond length is 1.46 Å. The S(1)-O(7) bond length is 1.49 Å. The S(1)-O(8) bond length is 1.51 Å. The S(1)-O(9) bond length is 1.49 Å. In the second S site, S(2) is bonded to one O(11), one O(12), one O(13), and one O(14) atom to form SO4 tetrahedra that share  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one Ni(2)O6 octahedra,  a cornercorner with one Ni(3)O5 square pyramid, and  a cornercorner with one Ni(4)O5 square pyramid. The corner-sharing octahedral tilt angles range from 53-55°. The S(2)-O(11) bond length is 1.49 Å. The S(2)-O(12) bond length is 1.47 Å. The S(2)-O(13) bond length is 1.50 Å. The S(2)-O(14) bond length is 1.48 Å. In the third S site, S(3) is bonded in a distorted single-bond geometry to one O(15) atom. The S(3)-O(15) bond length is 1.54 Å. In the fourth S site, S(4) is bonded in a distorted single-bond geometry to one C(11), one C(12), and one O(16) atom. The S(4)-O(16) bond length is 1.59 Å. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(4) and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(2) atom. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one Ni(4) and one C(2) atom. In the fifth O site, O(5) is bonded in a distorted single-bond geometry to one Ni(1), one Ni(2), one Ni(3), and one H(5) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Ni(2), one Ni(3), one Ni(4), and one H(6) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Ni(2) and one S(1) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Ni(3) and one S(1) atom. In the ninth O site, O(9) is bonded in a distorted trigonal planar geometry to one Ni(1), one Ni(4), and one S(1) atom. In the tenth O site, O(10) is bonded in a single-bond geometry to one S(1) atom. In the eleventh O site, O(11) is bonded in a distorted trigonal planar geometry to one Ni(1), one Ni(4), and one S(2) atom. In the twelfth O site, O(12) is bonded in a distorted bent 120 degrees geometry to one Ni(3) and one S(2) atom. In the thirteenth O site, O(13) is bonded in a single-bond geometry to one S(2) atom. In the fourteenth O site, O(14) is bonded in a bent 120 degrees geometry to one Ni(2) and one S(2) atom. In the fifteenth O site, O(15) is bonded in a distorted trigonal planar geometry to one Ni(1), one Ni(2), and one S(3) atom. In the sixteenth O site, O(16) is bonded in a distorted trigonal planar geometry to one Ni(1), one Ni(3), and one S(4) atom. Linkers: 6 [O]C(=O)c1cccc(C([O])=O)c1. Metal clusters: 1 C[S](C)O[Ni]1(O[S](C)C)O[C]O[Ni@@]2(O)O[C]O[Ni]3O[S@]([O])(O[Ni](O)O[S@@]([O])(O[Ni]4O[C]O[Ni@@]5(O)O[C]O[Ni](O[S](C)C)(O[S](C)C)O[S@]([O])(O[Ni](O)O[S@]([O])(O[Ni]6O[C]O[Ni@]7(O)O[C]O[Ni](O[S](C)C)(O[S](C)C)O[S@@]([O])(O[Ni](O)O[S@@]([O])(O[Ni]8O[C]O[Ni@@]9(O)O[C]O[Ni](O[S](C)C)(O[S](C)C)O[S@]([O])(O[Ni](O)O[S@]([O])(O[Ni]%10O[C]O[Ni@]%11(O)O[C]O[Ni](O[S](C)C)(O[S](C)C)O[S@@]([O])(O[Ni](O)O[S@@]([O])(O[Ni]%12O[C]O[Ni@@]%13(O)O[C]O[Ni](O[S](C)C)(O[S](C)C)O[S@]([O])(O[Ni](O)O[S@]([O])(O3)O%13)O%12)O%11)O%10)O9)O8)O7)O6)O5)O4)O2)O1. RCSR code: pcu. The MOF has largest included sphere 10.14 A, density 1.30 g/cm3, surface area 3232.73 m2/g, accessible volume 0.45 cm3/g