NiC13H9O6(CH3CO)2 crystallizes in the triclinic P-1 space group. The structure consists of eight dimethyl ether molecules inside a NiC13H9O6 framework. In the NiC13H9O6 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(1), one O(13), one O(14), one O(2), and two equivalent O(12) atoms to form a mixture of edge and corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 59-68°. The Ni(1)-O(1) bond length is 2.03 Å. The Ni(1)-O(13) bond length is 2.04 Å. The Ni(1)-O(14) bond length is 2.05 Å. The Ni(1)-O(2) bond length is 2.19 Å. There is one shorter (2.02 Å) and one longer (2.06 Å) Ni(1)-O(12) bond length. In the second Ni site, Ni(2) is bonded to one O(11), one O(12), one O(15), one O(16), one O(3), and one O(7) atom to form distorted corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 59-68°. The Ni(2)-O(11) bond length is 2.00 Å. The Ni(2)-O(12) bond length is 1.96 Å. The Ni(2)-O(15) bond length is 2.07 Å. The Ni(2)-O(16) bond length is 2.20 Å. The Ni(2)-O(3) bond length is 2.24 Å. The Ni(2)-O(7) bond length is 2.06 Å. There are twenty-six inequivalent C sites. In the first C site, C(33) is bonded in a distorted bent 120 degrees geometry to one C(30), one O(14), and one O(15) atom. The C(33)-C(30) bond length is 1.49 Å. The C(33)-O(14) bond length is 1.27 Å. The C(33)-O(15) bond length is 1.30 Å. In the second C site, C(34) is bonded in a distorted bent 120 degrees geometry to one C(32), one O(13), and one O(7) atom. The C(34)-C(32) bond length is 1.50 Å. The C(34)-O(13) bond length is 1.27 Å. The C(34)-O(7) bond length is 1.29 Å. In the third C site, C(1) is bonded in a distorted trigonal planar geometry to one C(10), one C(32), and one H(3) atom. The C(1)-C(10) bond length is 1.40 Å. The C(1)-C(32) bond length is 1.40 Å. The C(1)-H(3) bond length is 1.09 Å. In the fourth C site, C(2) is bonded in a trigonal planar geometry to one C(12), one C(3), and one C(4) atom. The C(2)-C(12) bond length is 1.43 Å. The C(2)-C(3) bond length is 1.41 Å. The C(2)-C(4) bond length is 1.44 Å. In the fifth C site, C(3) is bonded in a trigonal planar geometry to one C(10), one C(2), and one C(4) atom. The C(3)-C(10) bond length is 1.48 Å. The C(3)-C(4) bond length is 1.41 Å. In the sixth C site, C(4) is bonded in a trigonal planar geometry to one C(11), one C(2), and one C(3) atom. The C(4)-C(11) bond length is 1.43 Å. In the seventh C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(1), and one O(11) atom. The C(5)-C(6) bond length is 1.50 Å. The C(5)-O(1) bond length is 1.27 Å. The C(5)-O(11) bond length is 1.28 Å. In the eighth C site, C(6) is bonded in a trigonal planar geometry to one C(15), one C(5), and one C(8) atom. The C(6)-C(15) bond length is 1.40 Å. The C(6)-C(8) bond length is 1.40 Å. In the ninth C site, C(7) is bonded in a trigonal planar geometry to one C(13), one C(20), and one C(9) atom. The C(7)-C(13) bond length is 1.44 Å. The C(7)-C(20) bond length is 1.43 Å. The C(7)-C(9) bond length is 1.41 Å. In the tenth C site, C(8) is bonded in a distorted single-bond geometry to one C(14), one C(6), and one H(6) atom. The C(8)-C(14) bond length is 1.40 Å. The C(8)-H(6) bond length is 1.09 Å. In the eleventh C site, C(9) is bonded in a trigonal planar geometry to one C(13), one C(14), and one C(7) atom. The C(9)-C(13) bond length is 1.41 Å. The C(9)-C(14) bond length is 1.48 Å. In the twelfth C site, C(10) is bonded in a trigonal planar geometry to one C(1), one C(29), and one C(3) atom. The C(10)-C(29) bond length is 1.40 Å. In the thirteenth C site, C(11) is bonded in a distorted single-bond geometry to one C(4) and one H(7) atom. The C(11)-H(7) bond length is 1.09 Å. In the fourteenth C site, C(12) is bonded in a distorted single-bond geometry to one C(2) and one H(8) atom. The C(12)-H(8) bond length is 1.09 Å. In the fifteenth C site, C(13) is bonded in a trigonal planar geometry to one C(19), one C(7), and one C(9) atom. The C(13)-C(19) bond length is 1.43 Å. In the sixteenth C site, C(14) is bonded in a trigonal planar geometry to one C(17), one C(8), and one C(9) atom. The C(14)-C(17) bond length is 1.40 Å. In the seventeenth C site, C(15) is bonded in a distorted trigonal planar geometry to one C(27), one C(6), and one H(9) atom. The C(15)-C(27) bond length is 1.40 Å. The C(15)-H(9) bond length is 1.09 Å. In the eighteenth C site, C(17) is bonded in a distorted trigonal planar geometry to one C(14), one C(27), and one H(10) atom. The C(17)-C(27) bond length is 1.40 Å. The C(17)-H(10) bond length is 1.09 Å. In the nineteenth C site, C(19) is bonded in a single-bond geometry to one C(13) and one H(11) atom. The C(19)-H(11) bond length is 1.09 Å. In the twentieth C site, C(20) is bonded in a distorted single-bond geometry to one C(7) and one H(12) atom. The C(20)-H(12) bond length is 1.09 Å. In the twenty-first C site, C(21) is bonded in a distorted bent 120 degrees geometry to one C(27), one O(10), and one O(9) atom. The C(21)-C(27) bond length is 1.48 Å. The C(21)-O(10) bond length is 1.22 Å. The C(21)-O(9) bond length is 1.37 Å. In the twenty-second C site, C(27) is bonded in a trigonal planar geometry to one C(15), one C(17), and one C(21) atom. In the twenty-third C site, C(29) is bonded in a distorted single-bond geometry to one C(10), one C(30), and one H(26) atom. The C(29)-C(30) bond length is 1.40 Å. The C(29)-H(26) bond length is 1.09 Å. In the twenty-fourth C site, C(30) is bonded in a trigonal planar geometry to one C(29), one C(31), and one C(33) atom. The C(30)-C(31) bond length is 1.40 Å. In the twenty-fifth C site, C(31) is bonded in a distorted trigonal planar geometry to one C(30), one C(32), and one H(27) atom. The C(31)-C(32) bond length is 1.40 Å. The C(31)-H(27) bond length is 1.09 Å. In the twenty-sixth C site, C(32) is bonded in a trigonal planar geometry to one C(1), one C(31), and one C(34) atom. There are eighteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(2) atom. The H(1)-O(2) bond length is 0.97 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(2) atom. The H(2)-O(2) bond length is 1.00 Å. In the third H site, H(3) is bonded in a single-bond geometry to one C(1) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(3) atom. The H(4)-O(3) bond length is 0.98 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(3) atom. The H(5)-O(3) bond length is 0.98 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(8) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(11) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(12) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(15) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(17) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(19) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(20) atom. In the thirteenth H site, H(16) is bonded in a single-bond geometry to one O(9) atom. The H(16)-O(9) bond length is 0.98 Å. In the fourteenth H site, H(26) is bonded in a single-bond geometry to one C(29) atom. In the fifteenth H site, H(27) is bonded in a single-bond geometry to one C(31) atom. In the sixteenth H site, H(28) is bonded in a single-bond geometry to one O(12) atom. The H(28)-O(12) bond length is 0.98 Å. In the seventeenth H site, H(29) is bonded in a single-bond geometry to one O(16) atom. The H(29)-O(16) bond length is 0.98 Å. In the eighteenth H site, H(30) is bonded in a single-bond geometry to one O(16) atom. The H(30)-O(16) bond length is 0.98 Å. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(5) atom. In the second O site, O(2) is bonded in a distorted water-like geometry to one Ni(1), one H(1), and one H(2) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one Ni(2), one H(4), and one H(5) atom. In the fourth O site, O(7) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(34) atom. In the fifth O site, O(9) is bonded in a water-like geometry to one C(21) and one H(16) atom. In the sixth O site, O(10) is bonded in a single-bond geometry to one C(21) atom. In the seventh O site, O(11) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(5) atom. In the eighth O site, O(12) is bonded in a distorted single-bond geometry to one Ni(2), two equivalent Ni(1), and one H(28) atom. In the ninth O site, O(13) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(34) atom. In the tenth O site, O(14) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(33) atom. In the eleventh O site, O(15) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(33) atom. In the twelfth O site, O(16) is bonded in a distorted water-like geometry to one Ni(2), one H(29), and one H(30) atom. Linkers: 1 COc1cc2c(-c3cc(C([O])=O)cc(C([O])=O)c3)c3cc(OC)c(OC)cc3c(-c3cc(C([O])=O)cc(C([O])=O)c3)c2cc1OC ,2 [CH2]Oc1cc2c(-c3cc(C([O])=O)cc(C(=O)O)c3)c3cc(OC)c(OC)cc3c(-c3cc(C([O])=O)cc(C(=O)O)c3)c2cc1OC ,1 COc1cc2c(-c3cc(C([O])=O)cc(C(=O)O)c3)c3cc(OC)c(OC)cc3c(-c3cc(C([O])=O)cc(C(=O)O)c3)c2cc1OC. Metal clusters: 1 O.O.O.O.O.O.O[Ni@]12O[C]O[Ni](O[C]O1)O[C]O[Ni@]1(O)O[C]O[Ni](O[C]O2)O[C]O1. RCSR code: fsc. The MOF has largest included sphere 5.74 A, density 1.04 g/cm3, surface area 4569.53 m2/g, accessible volume 0.43 cm3/g