PRECURSORS OF HEXA-AZAMACROCYCLES. SYNTHESIS AND X-RAY STRUCTURE OF 2,9-DIAMINOPHENANTHROLINEBISACETATE-Co(II) AND 6,6'-DIAMINOBIPYRIDINE-BISACETATE-M(II) (M = Ni, Cu)
Titel:
PRECURSORS OF HEXA-AZAMACROCYCLES. SYNTHESIS AND X-RAY STRUCTURE OF 2,9-DIAMINOPHENANTHROLINEBISACETATE-Co(II) AND 6,6'-DIAMINOBIPYRIDINE-BISACETATE-M(II) (M = Ni, Cu)
Auteur:
Costamagna, Juan Caruso, Francesco Rossi, Miriam Campos, Marcelo Canales, Juan Ramirez, Juan
Verschenen in:
Journal of coordination chemistry
Paginering:
Jaargang 54 (2001) nr. 3-4 pagina's 247-259
Jaar:
2001-11-01
Inhoud:
The synthesis, conventional characterisations and x-ray structures of the following monomeric complexes are given for 2,9-diaminophenanthroline-bisacetate-cobalt(II) (A) and 6,6'-diaminobipyridine-bisacetate-M(II) (M = nickel(C) and copper(B)). Complex A crystalizes in the monoclinic, C2/c space group with a=12.813(6), b = 10.218(3), c= 13.811(5), Å; β= 118.17(2)°; Z=4; V=1549(2) Å3. A total of 1787 unique reflections with F > 6σ(F) were refined to values of R and Rw 0.0461 and 0.0774, respectively. Complex B crystallizes in the triclinic, P-1 space group with a=10.099(5), b=10.257(5), c=8.015(11), Å; α=112.98(2), β=93.13(2), γ=92.960(2),°; Z=2; V = 761(1), Å3. A total of 2603 unique reflections with F > 3.00σ(F) were refined to values of R and Rw 0.0764 and 0.1022, respectively. Complex C crystallizes in the monoclinic, P21/n space group with a=8.124(5), b=10.343(6), c=18.724(11), β=98.36(2),°; Z=4; V=1556(1), Å3. A total of 2537 unique reflections with F > 3.00σ(F) were refined to values of R and Rw 0.0689 and 0.0975, respectively. The structures consist of six-coordinate [M(CH3COO)2(L)] (L=2,9-diaminophenanthroline or 6,6'-diaminobipyridine) discrete monomeric neutral species, although in the Cu(II) compound the elongation of two long Cu—O bonds, due to the Jahn-Teller effect, makes the metal essentially four-coordinate. In the Ni and Co compounds the acetate acts as a bidentate ligand. The diamino ligands are coordinated by the pyridine nitrogen atoms. The IR spectra of the complexes have been recorded and are discussed in relation to the crystal structure and the acetate coordination mode.