Ag3GaC39H27(NO)6(Ag3GaC36H24(NO)6)2(CH)6 crystallizes in the trigonal R3c space group. The structure consists of thirty-six 02329_fluka molecules, two Ag3GaC36H24(NO)6 frameworks, and one Ag3GaC39H27(NO)6 framework. In one of the Ag3GaC36H24(NO)6 frameworks, Ag(2) is bonded in a linear geometry to one N(3) and one N(4) atom. The Ag(2)-N(3) bond length is 2.15 Å. The Ag(2)-N(4) bond length is 2.15 Å. Ga(2) is bonded in an octahedral geometry to three equivalent O(3) and three equivalent O(4) atoms. All Ga(2)-O(3) bond lengths are 1.94 Å. All Ga(2)-O(4) bond lengths are 1.96 Å. There are twelve inequivalent C sites. In the first C site, C(18) is bonded in a distorted single-bond geometry to one C(17), one C(19), and one H(12) atom. The C(18)-C(17) bond length is 1.39 Å. The C(18)-C(19) bond length is 1.39 Å. The C(18)-H(12) bond length is 0.95 Å. In the second C site, C(19) is bonded in a trigonal planar geometry to one C(14), one C(18), and one C(20) atom. The C(19)-C(14) bond length is 1.54 Å. The C(19)-C(20) bond length is 1.39 Å. In the third C site, C(20) is bonded in a single-bond geometry to one C(19), one C(21), and one H(13) atom. The C(20)-C(21) bond length is 1.39 Å. The C(20)-H(13) bond length is 0.95 Å. In the fourth C site, C(21) is bonded in a distorted trigonal planar geometry to one C(20), one N(3), and one H(14) atom. The C(21)-N(3) bond length is 1.39 Å. The C(21)-H(14) bond length is 0.95 Å. In the fifth C site, C(22) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(15) atom. The C(22)-N(4) bond length is 1.39 Å. The C(22)-H(15) bond length is 0.95 Å. In the sixth C site, C(23) is bonded in a distorted single-bond geometry to one C(24) and one H(16) atom. The C(23)-C(24) bond length is 1.39 Å. The C(23)-H(16) bond length is 0.95 Å. In the seventh C site, C(24) is bonded in a trigonal planar geometry to one C(16), one C(23), and one C(25) atom. The C(24)-C(16) bond length is 1.55 Å. The C(24)-C(25) bond length is 1.39 Å. In the eighth C site, C(25) is bonded in a distorted single-bond geometry to one C(24), one C(26), and one H(17) atom. The C(25)-C(26) bond length is 1.39 Å. The C(25)-H(17) bond length is 0.95 Å. In the ninth C site, C(26) is bonded in a distorted trigonal planar geometry to one C(25), one N(4), and one H(18) atom. The C(26)-N(4) bond length is 1.39 Å. The C(26)-H(18) bond length is 0.95 Å. In the tenth C site, C(14) is bonded in a distorted single-bond geometry to one C(19) and one O(3) atom. The C(14)-O(3) bond length is 1.32 Å. In the eleventh C site, C(16) is bonded in a distorted single-bond geometry to one C(24) and one O(4) atom. The C(16)-O(4) bond length is 1.27 Å. In the twelfth C site, C(17) is bonded in a distorted trigonal planar geometry to one C(18), one N(3), and one H(11) atom. The C(17)-N(3) bond length is 1.39 Å. The C(17)-H(11) bond length is 0.95 Å. There are two inequivalent N sites. In the first N site, N(3) is bonded in a trigonal planar geometry to one Ag(2), one C(17), and one C(21) atom. In the second N site, N(4) is bonded in a trigonal planar geometry to one Ag(2), one C(22), and one C(26) atom. There are eight inequivalent H sites. In the first H site, H(12) is bonded in a single-bond geometry to one C(18) atom. In the second H site, H(13) is bonded in a single-bond geometry to one C(20) atom. In the third H site, H(14) is bonded in a single-bond geometry to one C(21) atom. In the fourth H site, H(15) is bonded in a single-bond geometry to one C(22) atom. In the fifth H site, H(16) is bonded in a single-bond geometry to one C(23) atom. In the sixth H site, H(17) is bonded in a single-bond geometry to one C(25) atom. In the seventh H site, H(18) is bonded in a single-bond geometry to one C(26) atom. In the eighth H site, H(11) is bonded in a single-bond geometry to one C(17) atom. There are two inequivalent O sites. In the first O site, O(3) is bonded in a bent 120 degrees geometry to one Ga(2) and one C(14) atom. In the second O site, O(4) is bonded in a bent 120 degrees geometry to one Ga(2) and one C(16) atom. In one of the Ag3GaC36H24(NO)6 frameworks, Ag(3) is bonded in a linear geometry to one N(5) and one N(6) atom. The Ag(3)-N(5) bond length is 2.18 Å. The Ag(3)-N(6) bond length is 2.16 Å. Ga(3) is bonded in an octahedral geometry to three equivalent O(5) and three equivalent O(6) atoms. All Ga(3)-O(5) bond lengths are 1.91 Å. All Ga(3)-O(6) bond lengths are 1.95 Å. There are twelve inequivalent C sites. In the first C site, C(27) is bonded in a distorted single-bond geometry to one C(32) and one O(5) atom. The C(27)-C(32) bond length is 1.52 Å. The C(27)-O(5) bond length is 1.47 Å. In the second C site, C(29) is bonded in a distorted single-bond geometry to one C(37) and one O(6) atom. The C(29)-C(37) bond length is 1.45 Å. The C(29)-O(6) bond length is 1.32 Å. In the third C site, C(30) is bonded in a distorted trigonal planar geometry to one C(31), one N(5), and one H(20) atom. The C(30)-C(31) bond length is 1.39 Å. The C(30)-N(5) bond length is 1.39 Å. The C(30)-H(20) bond length is 0.95 Å. In the fourth C site, C(31) is bonded in a distorted single-bond geometry to one C(30), one C(32), and one H(21) atom. The C(31)-C(32) bond length is 1.39 Å. The C(31)-H(21) bond length is 0.95 Å. In the fifth C site, C(32) is bonded in a trigonal planar geometry to one C(27), one C(31), and one C(33) atom. The C(32)-C(33) bond length is 1.39 Å. In the sixth C site, C(33) is bonded in a single-bond geometry to one C(32), one C(34), and one H(22) atom. The C(33)-C(34) bond length is 1.39 Å. The C(33)-H(22) bond length is 0.95 Å. In the seventh C site, C(34) is bonded in a distorted trigonal planar geometry to one C(33), one N(5), and one H(23) atom. The C(34)-N(5) bond length is 1.39 Å. The C(34)-H(23) bond length is 0.95 Å. In the eighth C site, C(35) is bonded in a distorted trigonal planar geometry to one C(36), one N(6), and one H(24) atom. The C(35)-C(36) bond length is 1.39 Å. The C(35)-N(6) bond length is 1.39 Å. The C(35)-H(24) bond length is 0.95 Å. In the ninth C site, C(36) is bonded in a distorted single-bond geometry to one C(35), one C(37), and one H(25) atom. The C(36)-C(37) bond length is 1.39 Å. The C(36)-H(25) bond length is 0.95 Å. In the tenth C site, C(37) is bonded in a trigonal planar geometry to one C(29), one C(36), and one C(38) atom. The C(37)-C(38) bond length is 1.39 Å. In the eleventh C site, C(38) is bonded in a distorted single-bond geometry to one C(37), one C(39), and one H(26) atom. The C(38)-C(39) bond length is 1.39 Å. The C(38)-H(26) bond length is 0.95 Å. In the twelfth C site, C(39) is bonded in a distorted trigonal planar geometry to one C(38), one N(6), and one H(27) atom. The C(39)-N(6) bond length is 1.39 Å. The C(39)-H(27) bond length is 0.95 Å. There are two inequivalent N sites. In the first N site, N(5) is bonded in a trigonal planar geometry to one Ag(3), one C(30), and one C(34) atom. In the second N site, N(6) is bonded in a trigonal planar geometry to one Ag(3), one C(35), and one C(39) atom. There are eight inequivalent H sites. In the first H site, H(20) is bonded in a single-bond geometry to one C(30) atom. In the second H site, H(21) is bonded in a single-bond geometry to one C(31) atom. In the third H site, H(22) is bonded in a single-bond geometry to one C(33) atom. In the fourth H site, H(23) is bonded in a single-bond geometry to one C(34) atom. In the fifth H site, H(24) is bonded in a single-bond geometry to one C(35) atom. In the sixth H site, H(25) is bonded in a single-bond geometry to one C(36) atom. In the seventh H site, H(26) is bonded in a single-bond geometry to one C(38) atom. In the eighth H site, H(27) is bonded in a single-bond geometry to one C(39) atom. There are two inequivalent O sites. In the first O site, O(5) is bonded in a bent 120 degrees geometry to one Ga(3) and one C(27) atom. In the second O site, O(6) is bonded in a bent 120 degrees geometry to one Ga(3) and one C(29) atom. In the Ag3GaC39H27(NO)6 framework, Ag(1) is bonded in a linear geometry to one N(1) and one N(2) atom. The Ag(1)-N(1) bond length is 2.18 Å. The Ag(1)-N(2) bond length is 2.14 Å. Ga(1) is bonded in an octahedral geometry to three equivalent O(1) and three equivalent O(2) atoms. All Ga(1)-O(1) bond lengths are 1.96 Å. All Ga(1)-O(2) bond lengths are 1.96 Å. There are thirteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(6), and one O(1) atom. The C(1)-C(2) bond length is 1.34 Å. The C(1)-C(6) bond length is 1.45 Å. The C(1)-O(1) bond length is 1.29 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one H(1) atom. The C(2)-C(3) bond length is 1.41 Å. The C(2)-H(1) bond length is 0.95 Å. In the third C site, C(3) is bonded in a single-bond geometry to one C(11), one C(2), and one O(2) atom. The C(3)-C(11) bond length is 1.48 Å. The C(3)-O(2) bond length is 1.28 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(5), one N(1), and one H(2) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-N(1) bond length is 1.39 Å. The C(4)-H(2) bond length is 0.95 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(4), one C(6), and one H(3) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-H(3) bond length is 0.95 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(1), one C(5), and one C(7) atom. The C(6)-C(7) bond length is 1.39 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(6) and one H(4) atom. The C(7)-H(4) bond length is 0.95 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(5) atom. The C(8)-N(1) bond length is 1.39 Å. The C(8)-H(5) bond length is 0.95 Å. In the ninth C site, C(9) is bonded in a distorted trigonal planar geometry to one C(10), one N(2), and one H(6) atom. The C(9)-C(10) bond length is 1.39 Å. The C(9)-N(2) bond length is 1.39 Å. The C(9)-H(6) bond length is 0.95 Å. In the tenth C site, C(10) is bonded in a single-bond geometry to one C(11), one C(9), and one H(7) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-H(7) bond length is 0.95 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(3) atom. The C(11)-C(12) bond length is 1.39 Å. In the twelfth C site, C(12) is bonded in a distorted single-bond geometry to one C(11), one C(13), and one H(8) atom. The C(12)-C(13) bond length is 1.39 Å. The C(12)-H(8) bond length is 0.95 Å. In the thirteenth C site, C(13) is bonded in a distorted trigonal planar geometry to one C(12), one N(2), and one H(9) atom. The C(13)-N(2) bond length is 1.39 Å. The C(13)-H(9) bond length is 0.95 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ag(1), one C(4), and one C(8) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ag(1), one C(13), and one C(9) atom. There are nine inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) 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(7) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(8) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(9) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(10) 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(13) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ga(1) and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ga(1) and one C(3) atom. Linkers: 12 [O]/C(=C\[C](O[Ga](O[C](/C=C(\[O])c1ccncc1)c1ccncc1)O[C](/C=C(\[O])c1ccncc1)c1ccncc1)c1ccncc1)c1ccncc1 ,6 O=C(/C=C(\O[Ga](O/C(=C\C(=O)c1ccncc1)c1ccncc1)O/C(=C\C(=O)c1ccncc1)c1ccncc1)c1ccncc1)c1ccncc1. Metal clusters: 54 [Ag]. The MOF has largest included sphere 11.21 A, density 0.98 g/cm3, surface area 3724.02 m2/g, accessible volume 0.59 cm3/g