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Stacked schiff base complexes. The structural characterization of M,N′-ethylenebis(1,1,1-triflouro-2,4-pentanedioneiminato)copper(II0 and N,N′-ethylenebis(1,1,1-triflouro-2,4-hexanedioneiminato)nickel(II), Cu[en(tfpd)2] and Ni[en(tfhd)2]

✍ Scribed by Harry C. Allen Jr; Gregory L. Hillhouse; Derek J. Hodgson

Publisher
Elsevier Science
Year
1979
Tongue
English
Weight
736 KB
Volume
37
Category
Article
ISSN
0020-1693

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✦ Synopsis

The crystal and molecular structures of the Schiff base complexes N,N'-ethylenebis(l,l,I-trijluoro-2,4pentanedionato)copper(H), Cu [en(tfpd)z], C'UC~~-H,,N,O,F,, and N,N'-ethylenebis(l,l,I-trifluoro-2-4hexanedioneiminato-nickel(H) Ni[en(tjhd)J, NiC14

-HJWzFs> have been determined from threedimensional counter X-ray data. The copper complex crystallizes in the monoclinic space group P2Jc in a cell of dimensions a = 10.665(5), b = 16.131(9), c = 9.050(4) A, /3 = 106.43(5)". Least-squares refinement of the structure has led to a final R factor (on F) of 0.043 using 2351 independent intensities. The nickel complex also crystallizes in space group P2& with a = 11.43417). b = 17.798(b), c = 8.741(7) A and /3 = 110.60(5)". Least-squares refinement of the structure, based on 1054 independent observations, has led to an R-factor (on F) of 0.

073. The coordination geometry around the metal centers in both complexes is distorted square planar, the angle between the two N-M-O planes being 13.2" in the copper complex and 8.5" in the nickel complex; these results are in contrast with those reported earlier for the nickel analog of the present copper complex, Ni[en-(tfpd)z], in which the geometry was undistorted square planar, The average Cu-N and Cu-0 bond lengths are 1.939(8) and 1.909(4) A, respectively, while the corresponding values for the Ni-N and

Ni-0 bonds in Ni[en(tjhd), ] are 1.843(9) and 1.857(8) & respectively. Both complexes form stacks in the crystals, leading to Cu-Cu and Ni-Ni separations of 4.62.5(2) and 4.39.5(3) A, respectively, with associated Cu-Cu-Cu and Ni-Ni-Ni angles of 156.14(2) and 167.74(8)", respectively. The reported EPR spectra of pure and doped complexes of this type are discussed in the light of their structures.

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