PubMed · 4883867
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W Kraus. 1967. [Bicylic cations].. https://pubmed.ncbi.nlm.nih.gov/4883867/
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(I): 4,7-Dichloro-1-cyano-N-isopropyltetracyclo-[4.2.0.0(2,5).0(3,8)] octane-4-carboxamide, C13H14Cl2N2O, M(r) = 285.17, orthorhombic, Fdd2, a = 34.012 (1), b = 15.791 (2), c = 10.899(1)A, Z = 16, D chi = 1.29 g cm-3, Cu K alpha (lambda = 1.5418 A), mu = 39.2 cm-1, F(000) = 2368, T = 293 K, 1504 reflections with I > 3 sigma(I), R = 0.042. (II): 4,7-Dichloro-N-isopropyl-10-oxo-9-oxatetracyclo [4.4.0.0(2,5).0(3,8)]decane-4-carboxamide, C13H15Cl2NO3, M(r) = 304.17, monoclinic, P2(1)/a, a = 9.902(2), b = 9.381(2), c = 15.174(2) A, beta = 103.25(1) degrees, Z = 4, D chi = 1.47 g cm-3, Cu K alpha (lambda = 1.5418 A), mu = 43.1 cm-1, F(000) = 632, 2107 reflections with I > 3 sigma(I), R = 0.036. (I) represents the first crystallographic example of a secocubane. The nonbonded distances (C4...C7) are 2.742 (5) and 2.717(3) A in (I) and (II). C--C distances in the cage portions of the molecules are typical of cubanes.
Compound (I): cis-dichloro[mu-[bis[mu-[[2,6-diacetylpyridine dioximato](2-)-O:O']]dihydroxodiphenyl-diborato](3-)]- mu- mithoxydiiron, [Fe2(C30H29B2N6-O6)Cl2(CH3O)], M(r) = 804.9, monoclinic, Cc, a = 21.228 (6), b = 8.020 (2), c = 20.865 (5) A, beta = 105.2 (1) degrees, V = 3428 (2) A3, Z = 4, Dx = 1.56 g cm-3, lambda(Mo K alpha) = 0.7107 A, mu = 10.6 cm-1, F(000) = 1648, T = 275 K, R = 0.055 for 3018 unique reflections. Compound (I) contains a pseudo-twofold axis relating the two pyridine dioxime groups bound to the Fe atoms. In addition, two O atoms from the phenylborate moieties bridge the iron atoms, as does a methoxide. The two Cl atoms are bound to the seven coordinate metals axial to the methoxide. Compound (II): cis-dichloro[mu-[bis[mu-[[2,6-diacetylpyridine dioximato](2-)-O:O']]dihydroxodiphenyldiborato](3-)]-mu- hydroxodiiron, [Fe2(C30H29B2N6-O6)Cl2(OH)].H2O.2C2H3N, M(r) = 891.0, monoclinic, P2(1)/n, a = 11.860 (2), b = 20.911 (5), c = 16.175 (3) A, beta = 92.88 (1) degrees, V = 4006 (3) A3, Z = 4, Dx = 1.48 g cm-3, lambda(Mo K alpha) = 0.7107 A, mu = 9.1 cm-1, F(000) = 1832, T = 275 K, R = 0.051 for 7034 unique reflections. Compound (II) contains a hydroxide group replacing the methoxide in compound (I). The crystals also contain two acetonitriles of solvation. The bond lengths in the complex and the hydrogen-bonding pattern in the crystals are consistent with one of the bridging borate O atoms being protonated.(ABSTRACT TRUNCATED AT 250 WORDS)
Decahydro-1,6:3,4-dimethano-3a-nitrocyclobuta [1,2:3,4]dicyclopentene-2,5-dione (II), C12-H11NO4, Mr = 233.2, monoclinic, P2(1)/n, a = 13.378 (7), b = 6.614 (1), c = 23.040 (15) A, beta = 92.53 (5) degrees, V = 2036.6 (4) A3, Z = 8, D chi = 1.521 g cm-3, Cu K alpha, lambda = 1.54178 A, mu = 9.3 cm-1, F(000) = 1312, T = 293 K, final R = 0.047, wR = 0.075 for 3075 reflections with I greater than 3 sigma(I). There are no unusually short intermolecular distances. A comparison of the molecular densities and packing coefficients of (I) [4]peristylane-1,5-dione with (II), indicates that the change in crystal density from (I) (1.415 g cm-3) to (II) (1.521 g cm-3) is the sole result of an increase in molecular density with NO2 substitution. The packing coefficients for (I) and (II) are identical.