CoNiC16H6O9 crystallizes in the triclinic P1 space group. There are four inequivalent Co sites. In the first Co site, Co(1) is bonded to one O(1), one O(16), one O(24), one O(27), and one O(9) atom to form CoO5 square pyramids that share  a cornercorner with one Co(2)O5 square pyramid,  a cornercorner with one Co(4)O5 square pyramid, and  an edgeedge with one Ni(1)O5 square pyramid. The Co(1)-O(1) bond length is 2.07 Å. The Co(1)-O(16) bond length is 2.08 Å. The Co(1)-O(24) bond length is 2.03 Å. The Co(1)-O(27) bond length is 2.08 Å. The Co(1)-O(9) bond length is 2.02 Å. In the second Co site, Co(2) is bonded to one O(12), one O(17), one O(2), one O(5), and one O(9) atom to form CoO5 square pyramids that share  a cornercorner with one Co(1)O5 square pyramid and  a cornercorner with one Ni(1)O5 square pyramid. The Co(2)-O(12) bond length is 2.05 Å. The Co(2)-O(17) bond length is 2.12 Å. The Co(2)-O(2) bond length is 2.04 Å. The Co(2)-O(5) bond length is 2.08 Å. The Co(2)-O(9) bond length is 2.00 Å. In the third Co site, Co(3) is bonded to one O(10), one O(18), one O(33), one O(36), and one O(7) atom to form CoO5 square pyramids that share  a cornercorner with one Ni(2)O5 square pyramid,  a cornercorner with one Ni(4)O5 square pyramid, and  an edgeedge with one Ni(3)O5 square pyramid. The Co(3)-O(10) bond length is 2.07 Å. The Co(3)-O(18) bond length is 2.02 Å. The Co(3)-O(33) bond length is 2.03 Å. The Co(3)-O(36) bond length is 2.08 Å. The Co(3)-O(7) bond length is 2.08 Å. In the fourth Co site, Co(4) is bonded to one O(20), one O(23), one O(27), one O(30), and one O(35) atom to form CoO5 square pyramids that share  a cornercorner with one Co(1)O5 square pyramid and  a cornercorner with one Ni(1)O5 square pyramid. The Co(4)-O(20) bond length is 2.04 Å. The Co(4)-O(23) bond length is 2.08 Å. The Co(4)-O(27) bond length is 2.00 Å. The Co(4)-O(30) bond length is 2.05 Å. The Co(4)-O(35) bond length is 2.12 Å. There are four inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(19), one O(27), one O(34), one O(6), and one O(9) atom to form NiO5 square pyramids that share  a cornercorner with one Co(2)O5 square pyramid,  a cornercorner with one Co(4)O5 square pyramid, and  an edgeedge with one Co(1)O5 square pyramid. The Ni(1)-O(19) bond length is 2.07 Å. The Ni(1)-O(27) bond length is 2.02 Å. The Ni(1)-O(34) bond length is 2.08 Å. The Ni(1)-O(6) bond length is 2.03 Å. The Ni(1)-O(9) bond length is 2.08 Å. In the second Ni site, Ni(2) is bonded to one O(11), one O(14), one O(18), one O(3), and one O(8) atom to form NiO5 square pyramids that share  a cornercorner with one Co(3)O5 square pyramid and  a cornercorner with one Ni(3)O5 square pyramid. The Ni(2)-O(11) bond length is 2.04 Å. The Ni(2)-O(14) bond length is 2.08 Å. The Ni(2)-O(18) bond length is 2.00 Å. The Ni(2)-O(3) bond length is 2.05 Å. The Ni(2)-O(8) bond length is 2.12 Å. In the third Ni site, Ni(3) is bonded to one O(15), one O(18), one O(25), one O(28), and one O(36) atom to form NiO5 square pyramids that share  a cornercorner with one Ni(2)O5 square pyramid,  a cornercorner with one Ni(4)O5 square pyramid, and  an edgeedge with one Co(3)O5 square pyramid. The Ni(3)-O(15) bond length is 2.03 Å. The Ni(3)-O(18) bond length is 2.08 Å. The Ni(3)-O(25) bond length is 2.08 Å. The Ni(3)-O(28) bond length is 2.07 Å. The Ni(3)-O(36) bond length is 2.02 Å. In the fourth Ni site, Ni(4) is bonded to one O(21), one O(26), one O(29), one O(32), and one O(36) atom to form NiO5 square pyramids that share  a cornercorner with one Co(3)O5 square pyramid and  a cornercorner with one Ni(3)O5 square pyramid. The Ni(4)-O(21) bond length is 2.05 Å. The Ni(4)-O(26) bond length is 2.12 Å. The Ni(4)-O(29) bond length is 2.04 Å. The Ni(4)-O(32) bond length is 2.08 Å. The Ni(4)-O(36) bond length is 2.00 Å. There are thirty-six inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.26 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1); one C(3,19,35,51); and one C(7,39) atom. The C(2)-C(3,19,35,51) bond length is 1.39 Å. The C(2)-C(7,39) bond length is 1.40 Å. In the third C site, C(3,19,35,51) is bonded in a single-bond geometry to one C(2); one C(4,20,36,52); and one H(1,7,13,19) atom. The C(3,19,35,51)-C(4,20,36,52) bond length is 1.39 Å. The C(3,19,35,51)-H(1,7,13,19) bond length is 0.93 Å. In the fourth C site, C(4,20,36,52) is bonded in a trigonal planar geometry to one C(3,19,35,51); one C(5,21,37,53); and one C(9,25,41,57) atom. The C(4,20,36,52)-C(5,21,37,53) bond length is 1.40 Å. The C(4,20,36,52)-C(9,25,41,57) bond length is 1.48 Å. In the fifth C site, C(5,21,37,53) is bonded in a distorted single-bond geometry to one C(4,20,36,52) and one H(2,8,14,20) atom. The C(5,21,37,53)-H(2,8,14,20) bond length is 0.93 Å. In the sixth C site, C(6,22,38,54) is bonded in a single-bond geometry to one C(7,39) and one H(3,9,15,21) atom. The C(6,22,38,54)-C(7,39) bond length is 1.39 Å. The C(6,22,38,54)-H(3,9,15,21) bond length is 0.93 Å. In the seventh C site, C(7,39) is bonded in a trigonal planar geometry to one C(2); one C(6,22,38,54); and one C(8,40) atom. The C(7,39)-C(8,40) bond length is 1.52 Å. In the eighth C site, C(8,40) is bonded in a distorted bent 120 degrees geometry to one C(7,39); one O(3); and one O(4,22) atom. The C(8,40)-O(3) bond length is 1.26 Å. The C(8,40)-O(4,22) bond length is 1.25 Å. In the ninth C site, C(9,25,41,57) is bonded in a trigonal planar geometry to one C(10,26,42,58); one C(14,30,46,62); and one C(4,20,36,52) atom. The C(9,25,41,57)-C(10,26,42,58) bond length is 1.40 Å. The C(9,25,41,57)-C(14,30,46,62) bond length is 1.40 Å. In the tenth C site, C(10,26,42,58) is bonded in a distorted single-bond geometry to one C(9,25,41,57) and one H(4,10,16,22) atom. The C(10,26,42,58)-H(4,10,16,22) bond length is 0.93 Å. In the eleventh C site, C(11,27,43,59) is bonded in a distorted single-bond geometry to one C(12) and one H(5,11,17,23) atom. The C(11,27,43,59)-C(12) bond length is 1.39 Å. The C(11,27,43,59)-H(5,11,17,23) bond length is 0.93 Å. In the twelfth C site, C(12) is bonded in a trigonal planar geometry to one C(11,27,43,59); one C(13); and one C(15) atom. The C(12)-C(13) bond length is 1.40 Å. The C(12)-C(15) bond length is 1.50 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(12); one C(14,30,46,62); and one C(16) atom. The C(13)-C(14,30,46,62) bond length is 1.39 Å. The C(13)-C(16) bond length is 1.51 Å. In the fourteenth C site, C(14,30,46,62) is bonded in a distorted single-bond geometry to one C(13); one C(9,25,41,57); and one H(6,12,18,24) atom. The C(14,30,46,62)-H(6,12,18,24) bond length is 0.93 Å. In the fifteenth C site, C(15) is bonded in a distorted bent 120 degrees geometry to one C(12), one O(5), and one O(6) atom. The C(15)-O(5) bond length is 1.26 Å. The C(15)-O(6) bond length is 1.25 Å. In the sixteenth C site, C(16) is bonded in a distorted bent 120 degrees geometry to one C(13), one O(7), and one O(8) atom. The C(16)-O(7) bond length is 1.25 Å. The C(16)-O(8) bond length is 1.27 Å. In the seventeenth C site, C(17) is bonded in a distorted bent 120 degrees geometry to one C(18), one O(10), and one O(11) atom. The C(17)-C(18) bond length is 1.50 Å. The C(17)-O(10) bond length is 1.25 Å. The C(17)-O(11) bond length is 1.26 Å. In the eighteenth C site, C(18) is bonded in a trigonal planar geometry to one C(17); one C(23,55); and one C(3,19,35,51) atom. The C(18)-C(23,55) bond length is 1.40 Å. The C(18)-C(3,19,35,51) bond length is 1.39 Å. In the nineteenth C site, C(23,55) is bonded in a trigonal planar geometry to one C(18); one C(24,56); and one C(6,22,38,54) atom. The C(23,55)-C(24,56) bond length is 1.52 Å. The C(23,55)-C(6,22,38,54) bond length is 1.39 Å. In the twentieth C site, C(24,56) is bonded in a distorted bent 120 degrees geometry to one C(23,55); one O(12); and one O(13,31) atom. The C(24,56)-O(12) bond length is 1.26 Å. The C(24,56)-O(13,31) bond length is 1.25 Å. In the twenty-first C site, C(28) is bonded in a trigonal planar geometry to one C(11,27,43,59); one C(29); and one C(31) atom. The C(28)-C(11,27,43,59) bond length is 1.39 Å. The C(28)-C(29) bond length is 1.40 Å. The C(28)-C(31) bond length is 1.50 Å. In the twenty-second C site, C(29) is bonded in a trigonal planar geometry to one C(14,30,46,62); one C(28); and one C(32) atom. The C(29)-C(14,30,46,62) bond length is 1.39 Å. The C(29)-C(32) bond length is 1.51 Å. In the twenty-third C site, C(31) is bonded in a distorted bent 120 degrees geometry to one C(28), one O(14), and one O(15) atom. The C(31)-O(14) bond length is 1.26 Å. The C(31)-O(15) bond length is 1.25 Å. In the twenty-fourth C site, C(32) is bonded in a distorted bent 120 degrees geometry to one C(29), one O(16), and one O(17) atom. The C(32)-O(16) bond length is 1.25 Å. The C(32)-O(17) bond length is 1.27 Å. In the twenty-fifth C site, C(33) is bonded in a distorted bent 120 degrees geometry to one C(34), one O(19), and one O(20) atom. The C(33)-C(34) bond length is 1.50 Å. The C(33)-O(19) bond length is 1.25 Å. The C(33)-O(20) bond length is 1.26 Å. In the twenty-sixth C site, C(34) is bonded in a trigonal planar geometry to one C(3,19,35,51); one C(33); and one C(7,39) atom. The C(34)-C(3,19,35,51) bond length is 1.39 Å. The C(34)-C(7,39) bond length is 1.40 Å. In the twenty-seventh C site, C(44) is bonded in a trigonal planar geometry to one C(11,27,43,59); one C(45); and one C(47) atom. The C(44)-C(11,27,43,59) bond length is 1.39 Å. The C(44)-C(45) bond length is 1.40 Å. The C(44)-C(47) bond length is 1.50 Å. In the twenty-eighth C site, C(45) is bonded in a trigonal planar geometry to one C(14,30,46,62); one C(44); and one C(48) atom. The C(45)-C(14,30,46,62) bond length is 1.39 Å. The C(45)-C(48) bond length is 1.51 Å. In the twenty-ninth C site, C(47) is bonded in a distorted bent 120 degrees geometry to one C(44), one O(23), and one O(24) atom. The C(47)-O(23) bond length is 1.26 Å. The C(47)-O(24) bond length is 1.25 Å. In the thirtieth C site, C(48) is bonded in a distorted bent 120 degrees geometry to one C(45), one O(25), and one O(26) atom. The C(48)-O(25) bond length is 1.25 Å. The C(48)-O(26) bond length is 1.27 Å. In the thirty-first C site, C(49) is bonded in a distorted bent 120 degrees geometry to one C(50), one O(28), and one O(29) atom. The C(49)-C(50) bond length is 1.50 Å. The C(49)-O(28) bond length is 1.25 Å. The C(49)-O(29) bond length is 1.26 Å. In the thirty-second C site, C(50) is bonded in a trigonal planar geometry to one C(23,55); one C(3,19,35,51); and one C(49) atom. The C(50)-C(23,55) bond length is 1.40 Å. The C(50)-C(3,19,35,51) bond length is 1.39 Å. In the thirty-third C site, C(60) is bonded in a trigonal planar geometry to one C(11,27,43,59); one C(61); and one C(63) atom. The C(60)-C(11,27,43,59) bond length is 1.39 Å. The C(60)-C(61) bond length is 1.40 Å. The C(60)-C(63) bond length is 1.50 Å. In the thirty-fourth C site, C(61) is bonded in a trigonal planar geometry to one C(14,30,46,62); one C(60); and one C(64) atom. The C(61)-C(14,30,46,62) bond length is 1.39 Å. The C(61)-C(64) bond length is 1.51 Å. In the thirty-fifth C site, C(63) is bonded in a distorted bent 120 degrees geometry to one C(60), one O(32), and one O(33) atom. The C(63)-O(32) bond length is 1.26 Å. The C(63)-O(33) bond length is 1.25 Å. In the thirty-sixth C site, C(64) is bonded in a distorted bent 120 degrees geometry to one C(61), one O(34), and one O(35) atom. The C(64)-O(34) bond length is 1.25 Å. The C(64)-O(35) bond length is 1.27 Å. There are six inequivalent H sites. In the first H site, H(1,7,13,19) is bonded in a single-bond geometry to one C(3,19,35,51) atom. In the second H site, H(2,8,14,20) is bonded in a single-bond geometry to one C(5,21,37,53) atom. In the third H site, H(3,9,15,21) is bonded in a single-bond geometry to one C(6,22,38,54) atom. In the fourth H site, H(4,10,16,22) is bonded in a single-bond geometry to one C(10,26,42,58) atom. In the fifth H site, H(5,11,17,23) is bonded in a single-bond geometry to one C(11,27,43,59) atom. In the sixth H site, H(6,12,18,24) is bonded in a single-bond geometry to one C(14,30,46,62) atom. There are thirty-four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Co(1) and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Co(2) 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(8,40) atom. In the fourth O site, O(4,22) is bonded in a single-bond geometry to one C(8,40) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one Co(2) and one C(15) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(15) atom. In the seventh O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Co(3) and one C(16) atom. In the eighth O site, O(8) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(16) atom. In the ninth O site, O(9) is bonded in a trigonal non-coplanar geometry to one Co(1), one Co(2), and one Ni(1) atom. In the tenth O site, O(10) is bonded in a distorted bent 120 degrees geometry to one Co(3) and one C(17) atom. In the eleventh O site, O(11) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(17) atom. In the twelfth O site, O(12) is bonded in a distorted bent 120 degrees geometry to one Co(2) and one C(24,56) atom. In the thirteenth O site, O(13,31) is bonded in a single-bond geometry to one C(24,56) atom. In the fourteenth O site, O(14) is bonded in a distorted bent 150 degrees geometry to one Ni(2) and one C(31) atom. In the fifteenth O site, O(15) is bonded in a bent 120 degrees geometry to one Ni(3) and one C(31) atom. In the sixteenth O site, O(16) is bonded in a distorted bent 120 degrees geometry to one Co(1) and one C(32) atom. In the seventeenth O site, O(17) is bonded in a distorted bent 120 degrees geometry to one Co(2) and one C(32) atom. In the eighteenth O site, O(18) is bonded in a trigonal non-coplanar geometry to one Co(3), one Ni(2), and one Ni(3) atom. In the nineteenth O site, O(19) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(33) atom. In the twentieth O site, O(20) is bonded in a bent 120 degrees geometry to one Co(4) and one C(33) atom. In the twenty-first O site, O(21) is bonded in a distorted bent 120 degrees geometry to one Ni(4) and one C(8,40) atom. The O(21)-C(8,40) bond length is 1.26 Å. In the twenty-second O site, O(23) is bonded in a distorted bent 150 degrees geometry to one Co(4) and one C(47) atom. In the twenty-third O site, O(24) is bonded in a bent 120 degrees geometry to one Co(1) and one C(47) atom. In the twenty-fourth O site, O(25) is bonded in a distorted bent 120 degrees geometry to one Ni(3) and one C(48) atom. In the twenty-fifth O site, O(26) is bonded in a distorted bent 120 degrees geometry to one Ni(4) and one C(48) atom. In the twenty-sixth O site, O(27) is bonded in a trigonal non-coplanar geometry to one Co(1), one Co(4), and one Ni(1) atom. In the twenty-seventh O site, O(28) is bonded in a distorted bent 120 degrees geometry to one Ni(3) and one C(49) atom. In the twenty-eighth O site, O(29) is bonded in a bent 120 degrees geometry to one Ni(4) and one C(49) atom. In the twenty-ninth O site, O(30) is bonded in a distorted bent 120 degrees geometry to one Co(4) and one C(24,56) atom. The O(30)-C(24,56) bond length is 1.26 Å. In the thirtieth O site, O(32) is bonded in a distorted bent 150 degrees geometry to one Ni(4) and one C(63) atom. In the thirty-first O site, O(33) is bonded in a bent 120 degrees geometry to one Co(3) and one C(63) atom. In the thirty-second O site, O(34) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(64) atom. In the thirty-third O site, O(35) is bonded in a distorted bent 120 degrees geometry to one Co(4) and one C(64) atom. In the thirty-fourth O site, O(36) is bonded in a trigonal non-coplanar geometry to one Co(3), one Ni(3), and one Ni(4) atom. Linkers: 4 [O]C(=O)c1ccc(-c2ccc(C([O])=O)c(C([O])=O)c2)cc1C([O])=O. Metal clusters: 1 O=[C]O[Co]123O[C]O[Co](O[C]O1)(O[C]O[Co]14(O[C]=O)O[C]O[Ni](O[C]O2)(O[C]O1)O4)O3 ,1 O=[C]O[Ni]123O[C]O[Co](O[C]O1)(O[C]O[Ni]14(O[C]=O)O[C]O[Ni](O[C]O2)(O[C]O1)O4)O3. RCSR code: scu. The MOF has largest included sphere 4.64 A, density 1.53 g/cm3, surface area 3346.76 m2/g, accessible volume 0.27 cm3/g