An introduction to crystal chemistry by Robert Crispin Evans

By Robert Crispin Evans

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The four Fe(III) sites are assigned as the four metal sites trans to the shared edge of a decametallate core. Magnetic studies show t h a t 68 has a diamagnetic ground state. A mixed-valent heptadecanuclear iron cage has also been reported by this group, as part of a series of general formula [Fe16MOlo(OH)1o (OuCPh)2o] (M = Fe, Mn or Co) (160); the cage with M = Fe(II) is shown in Fig. 27. These cages are formed in low yield from reactions of the mixed-valent triangle [Fe30(O2CPh)6(H20)2(MeCN)]; the {Fe17} cage results from hydrolysis of a solution of the triangle in MeCN (with some 67 also found), while the cages containing Mn or Co involved reaction with suitable metal salts prior to crystallization.

The structure of [FeloNa206(OH)4(O2CPh)lo(chp)6(H20)2(Me2CO)2] (155). ) variable t e m p e r a t u r e magnetic data difficult; however, Cano et al. have recently reported Monte Carlo studies t h a t allow exchange parameters to be calculated (11). c. 3 K to reorientation of the magnetization (11). The first undecanuclear iron cage, [FellO6(OH)6(O2CPh)15] (67), shown in Fig. 26, was also reported by the Lippard group (158). It is formed by controlled slow hydrolysis of a solution containing [Fe2OC16]2- and Na(O2CPh) in MeCN.

Magnetization studies suggest an S -- 6 ground state. The oldest octanuclear Fe(III) cage is also the iron cage with the most heavily studied magnetic properties. [Fes(O)2(OH)12(tacn)6] s+ (58) (tacn -- 1, 4,7-triazacyclononane), shown in Fig. 23, was first reported FIG. 23. The structure of [Fe8(O)2(OH)12(tacn)6]s+ (145). ) HIGH-NUCLEARITY 3d-METAL COMPLEXES 53 by Wieghardt and co-workers in 1984 (145). The cage was made by hydrolysis of[FeC13(tacn)] at pH 9 in the presence of bromide. The structure consists of a planar octanuclear iron core, bridged by two tt3-oxides and twelve t~2-hydroxides.

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