Mo4CoC12N9H12O7 crystallizes in the triclinic P-1 space group. There are four inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a distorted rectangular see-saw-like geometry to one N(1), one O(1), one O(2), and one O(3) atom. The Mo(1)-N(1) bond length is 2.21 Å. The Mo(1)-O(1) bond length is 1.88 Å. The Mo(1)-O(2) bond length is 2.19 Å. The Mo(1)-O(3) bond length is 2.15 Å. In the second Mo site, Mo(2) is bonded in a 5-coordinate geometry to one O(2), one O(3), one O(4), and two equivalent O(5) atoms. The Mo(2)-O(2) bond length is 1.90 Å. The Mo(2)-O(3) bond length is 2.15 Å. The Mo(2)-O(4) bond length is 1.76 Å. There is one shorter (1.95 Å) and one longer (2.46 Å) Mo(2)-O(5) bond length. In the third Mo site, Mo(3) is bonded in a 5-coordinate geometry to one O(3), one O(4), one O(5), one O(6), and one O(7) atom. The Mo(3)-O(3) bond length is 1.92 Å. The Mo(3)-O(4) bond length is 2.34 Å. The Mo(3)-O(5) bond length is 2.24 Å. The Mo(3)-O(6) bond length is 1.73 Å. The Mo(3)-O(7) bond length is 1.94 Å. In the fourth Mo site, Mo(4) is bonded in a 4-coordinate geometry to one O(1), one O(2), one O(5), and one O(7) atom. The Mo(4)-O(1) bond length is 1.99 Å. The Mo(4)-O(2) bond length is 2.32 Å. The Mo(4)-O(5) bond length is 2.21 Å. The Mo(4)-O(7) bond length is 1.95 Å. Co(1) is bonded in a T-shaped geometry to one N(4), one N(7), and one O(6) atom. The Co(1)-N(4) bond length is 2.11 Å. The Co(1)-N(7) bond length is 2.15 Å. The Co(1)-O(6) bond length is 2.15 Å. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(4) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(3) bond length is 1.39 Å. The C(1)-C(4) bond length is 1.54 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(7) atom. The C(2)-C(3) bond length is 1.42 Å. The C(2)-C(7) bond length is 1.48 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(1), one C(10), and one C(2) atom. The C(3)-C(10) bond length is 1.48 Å. In the fourth C site, C(4) is bonded in a 3-coordinate geometry to one C(1), one N(2), one H(1), and one H(2) atom. The C(4)-N(2) bond length is 1.47 Å. The C(4)-H(1) bond length is 0.97 Å. The C(4)-H(2) bond length is 0.97 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one N(1), one N(2), and one H(3) atom. The C(5)-N(1) bond length is 1.30 Å. The C(5)-N(2) bond length is 1.35 Å. The C(5)-H(3) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one N(1), one N(3), and one H(4) atom. The C(6)-N(1) bond length is 1.37 Å. The C(6)-N(3) bond length is 1.30 Å. The C(6)-H(4) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a 3-coordinate geometry to one C(2); one N(5); and two equivalent H(5,6) atoms. The C(7)-N(5) bond length is 1.49 Å. Both C(7)-H(5,6) bond lengths are 0.97 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one N(4), one N(5), and one H(7) atom. The C(8)-N(4) bond length is 1.30 Å. The C(8)-N(5) bond length is 1.32 Å. The C(8)-H(7) bond length is 0.93 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one N(4), one N(6), and one H(8) atom. The C(9)-N(4) bond length is 1.35 Å. The C(9)-N(6) bond length is 1.31 Å. The C(9)-H(8) bond length is 0.93 Å. In the tenth C site, C(10) is bonded in a 3-coordinate geometry to one C(3); one N(8); and two equivalent H(9,10) atoms. The C(10)-N(8) bond length is 1.44 Å. Both C(10)-H(9,10) bond lengths are 0.97 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one N(7), one N(8), and one H(11) atom. The C(11)-N(7) bond length is 1.31 Å. The C(11)-N(8) bond length is 1.32 Å. The C(11)-H(11) bond length is 0.93 Å. In the twelfth C site, C(12) is bonded in a trigonal planar geometry to one N(7), one N(9), and one H(12) atom. The C(12)-N(7) bond length is 1.38 Å. The C(12)-N(9) bond length is 1.31 Å. The C(12)-H(12) bond length is 0.93 Å. There are nine inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Mo(1), one C(5), and one C(6) atom. In the second N site, N(2) is bonded in a 2-coordinate geometry to one C(4), one C(5), and one N(3) atom. The N(2)-N(3) bond length is 1.38 Å. In the third N site, N(3) is bonded in a water-like geometry to one C(6) and one N(2) atom. In the fourth N site, N(4) is bonded in a distorted trigonal planar geometry to one Co(1), one C(8), and one C(9) atom. In the fifth N site, N(5) is bonded in a distorted trigonal planar geometry to one C(7), one C(8), and one N(6) atom. The N(5)-N(6) bond length is 1.35 Å. In the sixth N site, N(6) is bonded in a water-like geometry to one C(9) and one N(5) atom. In the seventh N site, N(7) is bonded in a distorted trigonal planar geometry to one Co(1), one C(11), and one C(12) atom. In the eighth N site, N(8) is bonded in a 3-coordinate geometry to one C(10), one C(11), and one N(9) atom. The N(8)-N(9) bond length is 1.35 Å. In the ninth N site, N(9) is bonded in a water-like geometry to one C(12) and one N(8) atom. There are ten 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(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(6) atom. In the fifth H site, H(5,6) is bonded in a single-bond geometry to one C(7) atom. In the sixth H site, H(7) is bonded in a single-bond geometry to one C(8) atom. In the seventh H site, H(8) is bonded in a single-bond geometry to one C(9) atom. In the eighth H site, H(9,10) is bonded in a single-bond geometry to one C(10) atom. In the ninth H site, H(11) is bonded in a single-bond geometry to one C(11) atom. In the tenth H site, H(12) is bonded in a single-bond geometry to one C(12) atom. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Mo(1) and one Mo(4) atom. In the second O site, O(2) is bonded in a distorted trigonal non-coplanar geometry to one Mo(1), one Mo(2), and one Mo(4) atom. In the third O site, O(3) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(2), and one Mo(3) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Mo(2) and one Mo(3) atom. In the fifth O site, O(5) is bonded in a distorted rectangular see-saw-like geometry to one Mo(3), one Mo(4), and two equivalent Mo(2) atoms. In the sixth O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Mo(3) and one Co(1) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Mo(3) and one Mo(4) atom. Linkers: 1 [CH]1N=C[N]N1Cc1c(CN2[CH]N=C[N]2)c(CN2[CH]N=C[N]2)c(Cn2cncn2)c(Cn2cncn2)c1CN1[CH]N=C[N]1. Metal clusters: 1 [Co]O[Mo@]12O[Mo]3O[Mo]O[Mo@]4(O[Mo]5O[Mo]O[Mo@](O3)(O1)O[Mo@](O[Co])(O5)O4)O2. The MOF has largest included sphere 4.09 A, density 1.91 g/cm3, surface area 2858.82 m2/g, accessible volume 0.20 cm3/g