Synthesis, Characterization, and Crystal Structure of a Hexaaza Macrocyclic Complex of Lutetium(III)

A compound of formula Lu(C22H26N6)(CH3COO)(OH)(ClO4)(CH3OH)(H2O)0,5 was obtained by the metal-templated cyclic condensation of 1,2-diaminoethane with 2,6-diacetylpyridine, and its structure was determined by a single-crystal X-ray diffraction analysis. The compound crystallized in the triclinic space group PI with Z = 2, in a unit cell having a = 13.051 (3) Å, b = 11.351 (2) Å, c = 11.400 (2) Å, α = 108.95 (3)°, β = 104.63 (3)°, and γ = 100.40 (3)°. Its structure was ionic, with the complex cation consisting of 9-coordinate Lu(III) linked to the six N-donor atoms of the C22H26N6 macrocycle, to a bidentate chelating acetate, and to either a water or methanol molecule. Noncoordinated OH- and ClO4- balanced the residual cationic charges; clathrated methanol was also present. Thermogravimetric measurements and NMR (1H and 13C) spectra showed the compound to be thermally stable in the solid state as well as inert toward metal release in solution. © 1986, American Chemical Society. All rights reserved.