Ni2C36N4H24S2O9Br2 crystallizes in the monoclinic Cc space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one N(1), one N(3), one O(1), one O(6), one O(7), and one O(9) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 64°. The Ni(1)-N(1) bond length is 2.05 Å. The Ni(1)-N(3) bond length is 2.05 Å. The Ni(1)-O(1) bond length is 2.07 Å. The Ni(1)-O(6) bond length is 2.05 Å. The Ni(1)-O(7) bond length is 2.05 Å. The Ni(1)-O(9) bond length is 2.07 Å. In the second Ni site, Ni(2) is bonded to one N(2), one N(4), one O(2), one O(5), one O(8), and one O(9) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 64°. The Ni(2)-N(2) bond length is 2.05 Å. The Ni(2)-N(4) bond length is 2.05 Å. The Ni(2)-O(2) bond length is 2.06 Å. The Ni(2)-O(5) bond length is 2.05 Å. The Ni(2)-O(8) bond length is 2.05 Å. The Ni(2)-O(9) bond length is 2.07 Å. There are twenty-five inequivalent C sites. In the first C site, C(13,14) is bonded in a distorted single-bond geometry to one C(11), one C(3), and one H(7) atom. The C(13,14)-C(11) bond length is 1.39 Å. The C(13,14)-C(3) bond length is 1.40 Å. The C(13,14)-H(7) bond length is 1.09 Å. In the second C site, C(15,16) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(5), and one O(7) atom. The C(15,16)-C(7) bond length is 1.51 Å. The C(15,16)-O(5) bond length is 1.27 Å. The C(15,16)-O(7) bond length is 1.27 Å. In the third C site, C(17,18) is bonded in a distorted trigonal planar geometry to one C(19), one N(3), and one H(9) atom. The C(17,18)-C(19) bond length is 1.39 Å. The C(17,18)-N(3) bond length is 1.34 Å. The C(17,18)-H(9) bond length is 1.09 Å. In the fourth C site, C(19) is bonded in a distorted single-bond geometry to one C(17,18); one C(21,22); and one H(11,12) atom. The C(19)-C(21,22) bond length is 1.40 Å. The C(19)-H(11,12) bond length is 1.09 Å. In the fifth C site, C(20) is bonded in a distorted single-bond geometry to one C(17,18); one C(21,22); and one H(11,12) atom. The C(20)-C(17,18) bond length is 1.39 Å. The C(20)-C(21,22) bond length is 1.40 Å. The C(20)-H(11,12) bond length is 1.09 Å. In the sixth C site, C(21,22) is bonded in a trigonal planar geometry to one C(19), one C(23), and one S(1) atom. The C(21,22)-C(23) bond length is 1.40 Å. The C(21,22)-S(1) bond length is 1.77 Å. In the seventh C site, C(23) is bonded in a distorted trigonal planar geometry to one C(21,22); one C(25,26); and one H(13,14) atom. The C(23)-C(25,26) bond length is 1.39 Å. The C(23)-H(13,14) bond length is 1.09 Å. In the eighth C site, C(24) is bonded in a distorted trigonal planar geometry to one C(21,22); one C(25,26); and one H(13,14) atom. The C(24)-C(21,22) bond length is 1.40 Å. The C(24)-C(25,26) bond length is 1.39 Å. The C(24)-H(13,14) bond length is 1.09 Å. In the ninth C site, C(25,26) is bonded in a distorted bent 120 degrees geometry to one C(23), one N(3), and one H(15) atom. The C(25,26)-N(3) bond length is 1.35 Å. The C(25,26)-H(15) bond length is 1.09 Å. In the tenth C site, C(27,28) is bonded in a distorted bent 120 degrees geometry to one C(29), one N(1), and one H(17) atom. The C(27,28)-C(29) bond length is 1.39 Å. The C(27,28)-N(1) bond length is 1.35 Å. The C(27,28)-H(17) bond length is 1.09 Å. In the eleventh C site, C(29) is bonded in a distorted trigonal planar geometry to one C(27,28); one C(31,32); and one H(19,20) atom. The C(29)-C(31,32) bond length is 1.40 Å. The C(29)-H(19,20) bond length is 1.09 Å. In the twelfth C site, C(30) is bonded in a distorted trigonal planar geometry to one C(27,28); one C(31,32); and one H(19,20) atom. The C(30)-C(27,28) bond length is 1.39 Å. The C(30)-C(31,32) bond length is 1.40 Å. The C(30)-H(19,20) bond length is 1.09 Å. In the thirteenth C site, C(31,32) is bonded in a trigonal planar geometry to one C(29), one C(33), and one S(1) atom. The C(31,32)-C(33) bond length is 1.40 Å. The C(31,32)-S(1) bond length is 1.77 Å. In the fourteenth C site, C(33) is bonded in a distorted trigonal planar geometry to one C(31,32); one C(35,36); and one H(21,22) atom. The C(33)-C(35,36) bond length is 1.39 Å. The C(33)-H(21,22) bond length is 1.09 Å. In the fifteenth C site, C(34) is bonded in a distorted trigonal planar geometry to one C(31,32); one C(35,36); and one H(21,22) atom. The C(34)-C(31,32) bond length is 1.40 Å. The C(34)-C(35,36) bond length is 1.39 Å. The C(34)-H(21,22) bond length is 1.09 Å. In the sixteenth C site, C(35,36) is bonded in a distorted trigonal planar geometry to one C(33); one N(1); and one H(23,24) atom. The C(35,36)-N(1) bond length is 1.35 Å. The C(35,36)-H(23,24) bond length is 1.09 Å. In the seventeenth C site, C(1,2) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(1), and one O(3) atom. The C(1,2)-C(3) bond length is 1.51 Å. The C(1,2)-O(1) bond length is 1.28 Å. The C(1,2)-O(3) bond length is 1.27 Å. In the eighteenth C site, C(3) is bonded in a trigonal planar geometry to one C(1,2); one C(13,14); and one C(5,6) atom. The C(3)-C(5,6) bond length is 1.40 Å. In the nineteenth C site, C(4) is bonded in a trigonal planar geometry to one C(1,2); one C(13,14); and one C(5,6) atom. The C(4)-C(1,2) bond length is 1.51 Å. The C(4)-C(13,14) bond length is 1.40 Å. The C(4)-C(5,6) bond length is 1.40 Å. In the twentieth C site, C(5,6) is bonded in a distorted single-bond geometry to one C(3), one C(7), and one H(3) atom. The C(5,6)-C(7) bond length is 1.40 Å. The C(5,6)-H(3) bond length is 1.09 Å. In the twenty-first C site, C(7) is bonded in a trigonal planar geometry to one C(15,16); one C(5,6); and one C(9,10) atom. The C(7)-C(9,10) bond length is 1.40 Å. In the twenty-second C site, C(8) is bonded in a trigonal planar geometry to one C(15,16); one C(5,6); and one C(9,10) atom. The C(8)-C(15,16) bond length is 1.51 Å. The C(8)-C(5,6) bond length is 1.40 Å. The C(8)-C(9,10) bond length is 1.40 Å. In the twenty-third C site, C(9,10) is bonded in a distorted single-bond geometry to one C(11), one C(7), and one H(5) atom. The C(9,10)-C(11) bond length is 1.39 Å. The C(9,10)-H(5) bond length is 1.09 Å. In the twenty-fourth C site, C(11) is bonded in a trigonal planar geometry to one C(13,14); one C(9,10); and one Br(1,2) atom. The C(11)-Br(1,2) bond length is 1.92 Å. In the twenty-fifth C site, C(12) is bonded in a trigonal planar geometry to one C(13,14); one C(9,10); and one Br(1,2) atom. The C(12)-C(13,14) bond length is 1.39 Å. The C(12)-C(9,10) bond length is 1.39 Å. The C(12)-Br(1,2) bond length is 1.92 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(1); one C(27,28); and one C(35,36) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(2); one C(27,28); and one C(35,36) atom. The N(2)-C(27,28) bond length is 1.35 Å. The N(2)-C(35,36) bond length is 1.35 Å. In the third N site, N(3) is bonded in a trigonal planar geometry to one Ni(1); one C(17,18); and one C(25,26) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Ni(2); one C(17,18); and one C(25,26) atom. The N(4)-C(17,18) bond length is 1.34 Å. The N(4)-C(25,26) bond length is 1.35 Å. There are eighteen inequivalent H sites. In the first H site, H(1,2) is bonded in a distorted linear geometry to one O(3) and one O(9) atom. The H(1,2)-O(3) bond length is 1.52 Å. The H(1,2)-O(9) bond length is 1.04 Å. In the second H site, H(3) is bonded in a single-bond geometry to one C(5,6) atom. In the third H site, H(4) is bonded in a single-bond geometry to one C(5,6) atom. The H(4)-C(5,6) bond length is 1.09 Å. In the fourth H site, H(5) is bonded in a single-bond geometry to one C(9,10) atom. In the fifth H site, H(6) is bonded in a single-bond geometry to one C(9,10) atom. The H(6)-C(9,10) bond length is 1.09 Å. In the sixth H site, H(7) is bonded in a single-bond geometry to one C(13,14) atom. In the seventh H site, H(8) is bonded in a single-bond geometry to one C(13,14) atom. The H(8)-C(13,14) bond length is 1.09 Å. In the eighth H site, H(9) is bonded in a single-bond geometry to one C(17,18) atom. In the ninth H site, H(10) is bonded in a single-bond geometry to one C(17,18) atom. The H(10)-C(17,18) bond length is 1.09 Å. In the tenth H site, H(11,12) is bonded in a single-bond geometry to one C(19) atom. In the eleventh H site, H(13,14) is bonded in a single-bond geometry to one C(23) atom. In the twelfth H site, H(15) is bonded in a single-bond geometry to one C(25,26) atom. In the thirteenth H site, H(16) is bonded in a single-bond geometry to one C(25,26) atom. The H(16)-C(25,26) bond length is 1.09 Å. In the fourteenth H site, H(17) is bonded in a single-bond geometry to one C(27,28) atom. In the fifteenth H site, H(18) is bonded in a single-bond geometry to one C(27,28) atom. The H(18)-C(27,28) bond length is 1.09 Å. In the sixteenth H site, H(19,20) is bonded in a single-bond geometry to one C(29) atom. In the seventeenth H site, H(21,22) is bonded in a single-bond geometry to one C(33) atom. In the eighteenth H site, H(23,24) is bonded in a single-bond geometry to one C(35,36) atom. There are two inequivalent S sites. In the first S site, S(1) is bonded in a water-like geometry to one C(21,22) and one C(31,32) atom. In the second S site, S(2) is bonded in a water-like geometry to one C(21,22) and one C(31,32) atom. The S(2)-C(21,22) bond length is 1.77 Å. The S(2)-C(31,32) bond length is 1.77 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(1,2) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(1,2) atom. The O(2)-C(1,2) bond length is 1.28 Å. In the third O site, O(3) is bonded in a water-like geometry to one C(1,2) and one H(1,2) atom. In the fourth O site, O(4) is bonded in a water-like geometry to one C(1,2) and one H(1,2) atom. The O(4)-C(1,2) bond length is 1.27 Å. The O(4)-H(1,2) bond length is 1.52 Å. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(15,16) atom. In the sixth O site, O(8) is bonded in a distorted bent 150 degrees geometry to one Ni(2) and one C(15,16) atom. The O(8)-C(15,16) bond length is 1.27 Å. In the seventh O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(15,16) atom. The O(6)-C(15,16) bond length is 1.27 Å. In the eighth O site, O(9) is bonded in a distorted water-like geometry to one Ni(1); one Ni(2); and two equivalent H(1,2) atoms. In the ninth O site, O(7) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(15,16) atom. Br(1,2) is bonded in a single-bond geometry to one C(11) atom. Linkers: 4 [O]C(=O)c1cc(Br)cc(C([O])=O)c1 ,4 c1cc(Sc2ccncc2)ccn1. Metal clusters: 2 O.O=[C]O[Ni]1O[C]O[Ni](O[C]=O)O[C]O1. The MOF has largest included sphere 6.61 A, density 1.19 g/cm3, surface area 3754.68 m2/g, accessible volume 0.35 cm3/g