Rb3Co2H186(C25O4)6 crystallizes in the cubic I2_13 space group. Rb(1) is bonded in a 4-coordinate geometry to two equivalent O(1) and two equivalent O(2) atoms. Both Rb(1)-O(1) bond lengths are 2.74 Å. Both Rb(1)-O(2) bond lengths are 2.76 Å. Co(1) is bonded in a distorted T-shaped geometry to three equivalent O(4) atoms. All Co(1)-O(4) bond lengths are 2.04 Å. There are twenty-five inequivalent C sites. In the first C site, C(5) is bonded in a trigonal planar geometry to one C(16), one C(2), and one C(8) atom. The C(5)-C(16) bond length is 1.52 Å. The C(5)-C(2) bond length is 1.33 Å. The C(5)-C(8) bond length is 1.39 Å. In the second C site, C(6) is bonded in a distorted trigonal non-coplanar geometry to one H(2), one H(3), and one O(1) atom. The C(6)-H(2) bond length is 0.97 Å. The C(6)-H(3) bond length is 0.97 Å. The C(6)-O(1) bond length is 1.38 Å. In the third C site, C(7) is bonded in a tetrahedral geometry to one C(10), one C(19), one C(20), and one C(23) atom. The C(7)-C(10) bond length is 1.52 Å. The C(7)-C(19) bond length is 1.59 Å. The C(7)-C(20) bond length is 1.59 Å. The C(7)-C(23) bond length is 1.43 Å. In the fourth C site, C(8) is bonded in a distorted single-bond geometry to one C(14), one C(5), and one H(4) atom. The C(8)-C(14) bond length is 1.44 Å. The C(8)-H(4) bond length is 0.93 Å. In the fifth C site, C(9) is bonded in a trigonal planar geometry to one C(15), one C(18), and one C(2) atom. The C(9)-C(15) bond length is 1.41 Å. The C(9)-C(18) bond length is 1.44 Å. The C(9)-C(2) bond length is 1.37 Å. In the sixth C site, C(10) is bonded in a trigonal planar geometry to one C(12), one C(3), and one C(7) atom. The C(10)-C(12) bond length is 1.31 Å. The C(10)-C(3) bond length is 1.40 Å. In the seventh C site, C(11) is bonded in a trigonal planar geometry to one C(16), one C(3), and one C(4) atom. The C(11)-C(16) bond length is 1.57 Å. The C(11)-C(3) bond length is 1.31 Å. The C(11)-C(4) bond length is 1.41 Å. In the eighth C site, C(12) is bonded in a distorted single-bond geometry to one C(1), one C(10), and one H(5) atom. The C(12)-C(1) bond length is 1.42 Å. The C(12)-H(5) bond length is 0.98 Å. In the ninth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one O(2) and one O(4) atom. The C(13)-O(2) bond length is 1.19 Å. The C(13)-O(4) bond length is 1.34 Å. In the tenth C site, C(14) is bonded in a trigonal planar geometry to one C(15), one C(24), and one C(8) atom. The C(14)-C(15) bond length is 1.29 Å. The C(14)-C(24) bond length is 1.57 Å. In the eleventh C site, C(15) is bonded in a distorted single-bond geometry to one C(14), one C(9), and one H(6) atom. The C(15)-H(6) bond length is 0.93 Å. In the twelfth C site, C(16) is bonded in a water-like geometry to one C(11), one C(5), one H(7), and one H(8) atom. The C(16)-H(7) bond length is 0.97 Å. The C(16)-H(8) bond length is 0.97 Å. In the thirteenth C site, C(17) is bonded in a trigonal non-coplanar geometry to one C(24); one H(10); one H(11); and one H(9,20,22) atom. The C(17)-C(24) bond length is 1.64 Å. The C(17)-H(10) bond length is 0.96 Å. The C(17)-H(11) bond length is 0.96 Å. The C(17)-H(9,20,22) bond length is 0.96 Å. In the fourteenth C site, C(18) is bonded in a water-like geometry to one C(1), one C(9), one H(12), and one H(13) atom. The C(18)-C(1) bond length is 1.53 Å. The C(18)-H(12) bond length is 0.97 Å. The C(18)-H(13) bond length is 0.97 Å. In the fifteenth C site, C(19) is bonded in a trigonal non-coplanar geometry to one C(7); one H(16); and two equivalent H(14,15) atoms. The C(19)-H(16) bond length is 0.96 Å. Both C(19)-H(14,15) bond lengths are 0.96 Å. In the sixteenth C site, C(20) is bonded in a trigonal non-coplanar geometry to one C(7); one H(18); and two equivalent H(17,19) atoms. The C(20)-H(18) bond length is 0.96 Å. Both C(20)-H(17,19) bond lengths are 0.96 Å. In the seventeenth C site, C(21) is bonded in a trigonal non-coplanar geometry to one C(24); one H(21); and two equivalent H(9,20,22) atoms. The C(21)-C(24) bond length is 1.48 Å. The C(21)-H(21) bond length is 0.96 Å. Both C(21)-H(9,20,22) bond lengths are 0.96 Å. In the eighteenth C site, C(22) is bonded in a trigonal non-coplanar geometry to one C(24), one H(23), one H(24), and one H(25) atom. The C(22)-C(24) bond length is 1.44 Å. The C(22)-H(23) bond length is 0.96 Å. The C(22)-H(24) bond length is 0.96 Å. The C(22)-H(25) bond length is 0.96 Å. In the nineteenth C site, C(25) is bonded in a tetrahedral geometry to one H(29), one H(30), one H(31), and one O(3) atom. The C(25)-H(29) bond length is 0.96 Å. The C(25)-H(30) bond length is 0.96 Å. The C(25)-H(31) bond length is 0.96 Å. The C(25)-O(3) bond length is 1.25 Å. In the twentieth C site, C(23) is bonded in a trigonal non-coplanar geometry to one C(7), one H(26), one H(27), and one H(28) atom. The C(23)-H(26) bond length is 0.96 Å. The C(23)-H(27) bond length is 0.96 Å. The C(23)-H(28) bond length is 0.96 Å. In the twenty-first C site, C(24) is bonded in a tetrahedral geometry to one C(14), one C(17), one C(21), and one C(22) atom. In the twenty-second C site, C(1) is bonded in a trigonal planar geometry to one C(12), one C(18), and one C(4) atom. The C(1)-C(4) bond length is 1.42 Å. In the twenty-third C site, C(2) is bonded in a distorted trigonal planar geometry to one C(5), one C(9), and one O(1) atom. The C(2)-O(1) bond length is 1.41 Å. In the twenty-fourth C site, C(3) is bonded in a distorted single-bond geometry to one C(10), one C(11), and one H(1) atom. The C(3)-H(1) bond length is 0.98 Å. In the twenty-fifth C site, C(4) is bonded in a distorted single-bond geometry to one C(1), one C(11), and one O(3) atom. The C(4)-O(3) bond length is 1.37 Å. There are twenty-seven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(6) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(8) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(12) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(15) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(16) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(16) atom. In the ninth H site, H(9,20,22) is bonded in a single-bond geometry to one C(17) 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(17) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(18) atom. In the thirteenth H site, H(13) is bonded in a single-bond geometry to one C(18) atom. In the fourteenth H site, H(14,15) is bonded in a single-bond geometry to one C(19) atom. In the fifteenth H site, H(16) is bonded in a single-bond geometry to one C(19) atom. In the sixteenth H site, H(17,19) is bonded in a single-bond geometry to one C(20) atom. In the seventeenth H site, H(18) is bonded in a single-bond geometry to one C(20) atom. In the eighteenth H site, H(21) is bonded in a single-bond geometry to one C(21) atom. In the nineteenth H site, H(23) is bonded in a single-bond geometry to one C(22) atom. In the twentieth H site, H(24) is bonded in a single-bond geometry to one C(22) atom. In the twenty-first H site, H(25) is bonded in a single-bond geometry to one C(22) atom. In the twenty-second H site, H(26) is bonded in a single-bond geometry to one C(23) atom. In the twenty-third H site, H(27) is bonded in a single-bond geometry to one C(23) atom. In the twenty-fourth H site, H(28) is bonded in a single-bond geometry to one C(23) atom. In the twenty-fifth H site, H(29) is bonded in a single-bond geometry to one C(25) atom. In the twenty-sixth H site, H(30) is bonded in a single-bond geometry to one C(25) atom. In the twenty-seventh H site, H(31) is bonded in a single-bond geometry to one C(25) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one Rb(1), one C(2), and one C(6) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Rb(1) and one C(13) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one C(25) and one C(4) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Co(1) and one C(13) atom. Linkers: 12 COc1c2cc(C(C)(C)C)cc1Cc1cc(C(C)(C)C)cc(c1OCC([O])=O)Cc1cc(C(C)(C)C)cc(c1OC)Cc1cc(C(C)(C)C)cc(c1OCC([O])=O)C2. Metal clusters: 12 [Rb] ,8 [Co]. The MOF has largest included sphere 6.32 A, density 0.92 g/cm3, surface area 5252.11 m2/g, accessible volume 0.56 cm3/g