Mo8Ni3C16H22(N7O16)2(CH)2 crystallizes in the triclinic P-1 space group. The structure consists of two 02329_fluka molecules inside a Mo8Ni3C16H22(N7O16)2 framework. In the Mo8Ni3C16H22(N7O16)2 framework, there are four inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a 6-coordinate geometry to one O(1), one O(3), one O(4), one O(5), and two equivalent O(2) atoms. The Mo(1)-O(1) bond length is 1.90 Å. The Mo(1)-O(3) bond length is 1.73 Å. The Mo(1)-O(4) bond length is 2.21 Å. The Mo(1)-O(5) bond length is 1.75 Å. There is one shorter (1.92 Å) and one longer (2.57 Å) Mo(1)-O(2) bond length. In the second Mo site, Mo(2) is bonded in a 6-coordinate geometry to one N(1), one O(1), one O(4), one O(6), one O(7), and one O(8) atom. The Mo(2)-N(1) bond length is 2.21 Å. The Mo(2)-O(1) bond length is 2.26 Å. The Mo(2)-O(4) bond length is 2.06 Å. The Mo(2)-O(6) bond length is 1.74 Å. The Mo(2)-O(7) bond length is 1.76 Å. The Mo(2)-O(8) bond length is 1.86 Å. In the third Mo site, Mo(3) is bonded in a 6-coordinate geometry to one O(1), one O(10), one O(11), one O(2), one O(8), and one O(9) atom. The Mo(3)-O(1) bond length is 2.41 Å. The Mo(3)-O(10) bond length is 1.71 Å. The Mo(3)-O(11) bond length is 1.95 Å. The Mo(3)-O(2) bond length is 2.27 Å. The Mo(3)-O(8) bond length is 1.98 Å. The Mo(3)-O(9) bond length is 1.72 Å. In the fourth Mo site, Mo(4) is bonded in a 6-coordinate geometry to one O(11), one O(12), one O(13), one O(2), one O(4), and one O(5) atom. The Mo(4)-O(11) bond length is 1.90 Å. The Mo(4)-O(12) bond length is 1.76 Å. The Mo(4)-O(13) bond length is 1.71 Å. The Mo(4)-O(2) bond length is 2.27 Å. The Mo(4)-O(4) bond length is 1.96 Å. The Mo(4)-O(5) bond length is 2.30 Å. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in an octahedral geometry to one N(2), one N(3), one O(14), one O(15), one O(6), and one O(7) atom. The Ni(1)-N(2) bond length is 2.09 Å. The Ni(1)-N(3) bond length is 2.08 Å. The Ni(1)-O(14) bond length is 2.04 Å. The Ni(1)-O(15) bond length is 2.09 Å. The Ni(1)-O(6) bond length is 2.04 Å. The Ni(1)-O(7) bond length is 2.02 Å. In the second Ni site, Ni(2) is bonded in an octahedral geometry to two equivalent N(4), two equivalent N(5), and two equivalent O(16) atoms. Both Ni(2)-N(4) bond lengths are 2.02 Å. Both Ni(2)-N(5) bond lengths are 2.23 Å. Both Ni(2)-O(16) bond lengths are 2.19 Å. There are eight inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(1), one N(4), and one H(1) atom. The C(1)-N(1) bond length is 1.33 Å. The C(1)-N(4) bond length is 1.34 Å. The C(1)-H(1) bond length is 1.09 Å. In the second C site, C(2) is bonded in a distorted water-like geometry to one C(3), one N(2), and one N(4) atom. The C(2)-C(3) bond length is 1.44 Å. The C(2)-N(2) bond length is 1.33 Å. The C(2)-N(4) bond length is 1.37 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(2), one N(5), and one N(6) atom. The C(3)-N(5) bond length is 1.34 Å. The C(3)-N(6) bond length is 1.35 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(5), one N(6), and one N(7) atom. The C(4)-C(5) bond length is 1.46 Å. The C(4)-N(6) bond length is 1.35 Å. The C(4)-N(7) bond length is 1.35 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(7) atom. The C(5)-C(6) bond length is 1.40 Å. The C(5)-C(7) bond length is 1.40 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5) and one H(9) atom. The C(6)-H(9) bond length is 1.09 Å. In the seventh C site, C(7) is bonded in a distorted trigonal planar geometry to one C(5), one N(3), and one H(10) atom. The C(7)-N(3) bond length is 1.34 Å. The C(7)-H(10) bond length is 1.09 Å. In the eighth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(12) atom. The C(9)-N(3) bond length is 1.35 Å. The C(9)-H(12) bond length is 1.09 Å. There are seven inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Mo(2), one C(1), and one N(2) atom. The N(1)-N(2) bond length is 1.37 Å. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Ni(1), one C(2), and one N(1) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Ni(1), one C(7), and one C(9) atom. In the fourth N site, N(4) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(1), and one C(2) atom. In the fifth N site, N(5) is bonded in a 3-coordinate geometry to one Ni(2), one C(3), and one N(7) atom. The N(5)-N(7) bond length is 1.35 Å. In the sixth N site, N(6) is bonded in a distorted trigonal non-coplanar geometry to one C(3), one C(4), and one H(3) atom. The N(6)-H(3) bond length is 1.70 Å. In the seventh N site, N(7) is bonded in a 2-coordinate geometry to one C(4), one N(5), and one H(8) atom. The N(7)-H(8) bond length is 1.06 Å. There are eleven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one O(14) atom. The H(2)-O(14) bond length is 0.98 Å. In the third H site, H(3) is bonded in a distorted single-bond geometry to one N(6) and one O(14) atom. The H(3)-O(14) bond length is 1.01 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(15) atom. The H(4)-O(15) bond length is 0.98 Å. In the fifth H site, H(5) is bonded in a distorted bent 150 degrees geometry to one O(1) and one O(15) atom. The H(5)-O(1) bond length is 1.68 Å. The H(5)-O(15) bond length is 1.00 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one O(16) atom. The H(6)-O(16) bond length is 0.97 Å. In the seventh H site, H(7) is bonded in a distorted single-bond geometry to one O(16) and one O(3) atom. The H(7)-O(16) bond length is 1.00 Å. The H(7)-O(3) bond length is 1.69 Å. In the eighth H site, H(8) is bonded in a linear geometry to one N(7) and one O(12) atom. The H(8)-O(12) bond length is 1.59 Å. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(6) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(7) atom. In the eleventh H site, H(12) is bonded in a single-bond geometry to one C(9) atom. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to one Mo(1), one Mo(2), one Mo(3), and one H(5) atom. In the second O site, O(2) is bonded in a 4-coordinate geometry to one Mo(3), one Mo(4), and two equivalent Mo(1) atoms. In the third O site, O(3) is bonded in a distorted linear geometry to one Mo(1) and one H(7) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(2), and one Mo(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Mo(1) and one Mo(4) atom. In the sixth O site, O(6) is bonded in a bent 150 degrees geometry to one Mo(2) and one Ni(1) atom. In the seventh O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Mo(2) and one Ni(1) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Mo(2) and one Mo(3) atom. In the ninth O site, O(9) is bonded in a single-bond geometry to one Mo(3) atom. In the tenth O site, O(10) is bonded in a single-bond geometry to one Mo(3) atom. In the eleventh O site, O(11) is bonded in a bent 120 degrees geometry to one Mo(3) and one Mo(4) atom. In the twelfth O site, O(12) is bonded in a bent 150 degrees geometry to one Mo(4) and one H(8) atom. In the thirteenth O site, O(13) is bonded in a single-bond geometry to one Mo(4) atom. In the fourteenth O site, O(14) is bonded in a distorted water-like geometry to one Ni(1), one H(2), and one H(3) atom. In the fifteenth O site, O(15) is bonded in a distorted trigonal non-coplanar geometry to one Ni(1), one H(4), and one H(5) atom. In the sixteenth O site, O(16) is bonded in a distorted trigonal non-coplanar geometry to one Ni(2), one H(6), and one H(7) atom. Linkers: 2 O.O.[CH]=[C]C1=NC2=C3N=N[CH]N3[Ni@]3(N4[CH]N=NC4=C4N=C(c5cccnc5)NN43)N2N1 ,1 O.O.[CH]1N=NC2=C3N=C(c4cccnc4)NN3[Ni]3(N12)N1[CH]N=NC1=C1N=C(c2cccnc2)NN13. Metal clusters: 2 [Ni] ,8 [Mo]. The MOF has largest included sphere 3.92 A, density 2.38 g/cm3, surface area 2249.85 m2/g, accessible volume 0.11 cm3/g