Template synthesis and crystal and molecular structure of bis[1,1,1,12,12,12-hexafluoro-2,11-bis(trifluoromethyl)-4,9-dimethyl-2,11-diolato-5,8-diazadodeca-4,8-diene(2-)]cerium(IV), CeC28H28F24O4N4. A fluorinated Schiff base complex of eight-coordinate cerium(IV)
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The synthesis and crystal and molecular structure of bis[l, l, l, 12, 12, 12-hexafluoro-2, ll-bis(trifluoromethyl)-4, 9-dimethyl-2, 1 l-diolate-5, 8-diazadodeca-4, 8-diene(2-)]cerium(IV), CeC28H28F2404N4, is described. The compound was prepared by template condensation of ethylenediamine and 5, 5, 5-trifluoro-4-hydroxy-4-trifluoromethyl-2-pentanone at an eight-coordinate center. The initial reaction mixture contains Ce(III), and the reaction involves both the template condensation and the oxidation of Ce(III) to Ce(IV); the order of these steps is uncertain. The pale yellow crystalline product is monoclinic and conforms to the space group P21/c. Cell constants are a = 19.881 (1) Å, b = 10.970 (1) Å, c = 17.605 (2) Å, β = 91.49 (2)°, V = 3838 (1) Å3, and Z = 4. Final refinement of the structure gave RF = 0.036, RwF = 0.057, and the error in an observation of unit weight is 1.760. The coordination sphere forms a distorted square antiprism, and the two ligands assume meridional configurations at ∼90° to one another. The Ce-0 distances range from 2.196 (2) to 2.230 (2) Å, and the Ce-N distances range from 2.609 (3) to 2.641 (3) Å (average 2.623 (6) Å). This is a novel cerium Schiff base complex and also the first report of Ce-N bonding. © 1980, American Chemical Society. All rights reserved.
author list (cited authors)
Timmons, J. H., Martin, J., Martell, A. E., Rudolf, P., Clearfield, A., Arner, J. H., Loeb, S. J., & Willis, C. J.