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Extra info for Advances in Inorganic Chemistry, Vol. 52

Example text

The synthetic procedure is quite different, involving addition of NEt4C1 to a tetranuclear manganese(III) butterfly, [Mn402(O2CMe)6(py)2(dbm)2] in CH2C12. This transformation is both solvent-dependent and difficult to rationalize; in MeCN, the same reaction gives [Mn403Cl(O2CMe)3(dbm)3] (91). Magnetic measurements indicate that 30 has a complicated spin structure, and it was not possible to conclude whether the ground state was S = 3 or S = 4 based on preliminary magnetization studies. A heptanuclear manganese(II) cage, [Mn706(OEt)ls(HOEt)2], has also been crystallized from the reaction of anhydrous MnC12 with NaSb(OEt)4 by controlled hydrolysis in toluene-ethanol (92).

A tridecanuclear cage, [Mn13Os(OEt)6(O2CPh)12] (49), has perhaps the most appealing structure (121), which is shown in Fig. 19. It is a supercubane, containing Mr i n Fro. 19. The structure of [Mn13Os(OEt)6(O2CPh)12] (121),with phenyl groups excluded for clarity. ) 46 WINPENNY eight cubanes arranged in a cube. The central manganese site is a Mn(IV) center, and is shared by all eight cubanes. The 12 surrounding Mn centers are half Mn(III) and half Mn(II), and can be assigned because the Mn(III) sites show a Jahn-Teller elongated coordination geometry.

Clearly the alkali metal is templating the formation of one cage rather than the other. With N-methyldiethanolamine, reaction with FeC13 in T H F in the presence of Cs2CO3 leads to an empty cage, [Fe6C16{OCH2CH2)2NMe}6] (140), with bridging between Fe centers similar to that in 56, but with six terminal chloride ligands attached to the six Fe sites. Use of a bis(bipyridine) ligand has also generated a hexanuclear iron(III) cage, [Fe604C14(O2CPh)4(L6)2] 2+ (141), where L6 = 1,2-bis(2,2'bipyridyl-6-yl)ethane.

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