NiC7H11S(NO2)2CH crystallizes in the orthorhombic Pmc2_1 space group. The structure consists of two 02329_fluka molecules inside a NiC7H11S(NO2)2 framework. In the NiC7H11S(NO2)2 framework, Ni(1) is bonded to two equivalent N(1), one O(1), one O(2), and two equivalent O(3) atoms to form NiN2O4 octahedra that share corners with two equivalent S(1)O4 tetrahedra and  an edgeedge with one S(1)O4 tetrahedra. Both Ni(1)-N(1) bond lengths are 2.04 Å. The Ni(1)-O(1) bond length is 2.14 Å. The Ni(1)-O(2) bond length is 2.09 Å. Both Ni(1)-O(3) bond lengths are 2.30 Å. There are four inequivalent C sites. In the first C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(2) atom. The C(3)-C(2) bond length is 1.40 Å. The C(3)-H(2) bond length is 1.09 Å. In the second C site, C(4) is bonded in a distorted trigonal non-coplanar geometry to one C(2), one N(1), one H(3), and one H(4) atom. The C(4)-C(2) bond length is 1.51 Å. The C(4)-N(1) bond length is 1.47 Å. The C(4)-H(3) bond length is 1.10 Å. The C(4)-H(4) bond length is 1.10 Å. In the third C site, C(5) is bonded in a distorted single-bond geometry to two equivalent C(2) and one H(5) atom. Both C(5)-C(2) bond lengths are 1.40 Å. The C(5)-H(5) bond length is 1.09 Å. In the fourth C site, C(2) is bonded in a trigonal planar geometry to one C(3), one C(4), and one C(5) atom. N(1) is bonded to one Ni(1), one C(4), one H(6), and one H(7) atom to form distorted corner-sharing NNiH2C tetrahedra. The N(1)-H(6) bond length is 1.03 Å. The N(1)-H(7) bond length is 1.02 Å. There are six inequivalent H sites. In the first H site, H(2) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(3) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(4) is bonded in a single-bond geometry to one C(4) atom. In the fourth H site, H(5) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(6) is bonded in a single-bond geometry to one N(1) atom. In the sixth H site, H(7) is bonded in a single-bond geometry to one N(1) atom. S(1) is bonded to one O(1), one O(2), and two equivalent O(3) atoms to form SO4 tetrahedra that share corners with two equivalent Ni(1)N2O4 octahedra and  an edgeedge with one Ni(1)N2O4 octahedra. The corner-sharing octahedral tilt angles range from 50-53°. The S(1)-O(1) bond length is 1.49 Å. The S(1)-O(2) bond length is 1.50 Å. Both S(1)-O(3) bond lengths are 1.50 Å. There are three inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one S(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one S(1) atom. In the third O site, O(3) is bonded in a distorted L-shaped geometry to one Ni(1) and one S(1) atom. Linkers: 2 [O]S([O])(=O)=O. Metal clusters: 2 [Ni]. The MOF has largest included sphere 2.16 A, density 1.91 g/cm3, surface area 3340.18 m2/g, accessible volume 0.09 cm3/g