Synthesis of homodinuclear macrocyclic complexes of lanthanides and phenolic schiff bases

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Successful syntheses of the first examples of homodinuclear macrocyclic lanthanide complexes are reported. The complexes were obtained as compounds of the 2:2 Schiff base formed by condensing 2,6-diformyl-p-cresol and triethylenetetramine (L7) by a template procedure using lanthanide nitrates and perchlorates. When reactant methanolic solutions were concentrated the complexes were deposited as yellow or orange microcrystalline precipitates, Ln2L7(NO3)4sigma; nH2O or Ln2L7(NO3)4tau; x(OH)x, x = 1 or 2, whereas solutions diluted three times deposited complexes as flaky off-white crystalline precipitates of light lanthanides. The orange Ln2L7(NO3)2(OH)2 complexes can be converted in quantitative yield to the off-white flaky form of Ln2L7(NO3)4sigma; nH2O by refluxing them in methanolic solution containing triethylenetetramine and a three-fold excess of Ln(NO3)3. The complexes were characterized by elemental analysis, fast atom bombardment mass spectrometry, UV-Vis and infrared spectroscopy and thermogravimetry. Interesting and mostly new polyatomic oxo clusters, e.g. Ln2O3+, Ln3O4+, Ln4O6+, Ln5O7+, were dominant in the mass spectra but are treated in detail elsewhere. © 1986.

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Inorganica Chimica Acta

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