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Anion encapsulation promoted by anion?π interactions in rationally designed hexanuclear antiferromagnetic wheels: synthesis, structure and magnetic properties
Corresponding authors
Departamento de Química Inorgánica, Universidad de Granada, Av. Fuentenueva S/N, Granada, Spain
Département de Chimie, Université Abdelmalek Essaadi, Faculté des Sciences, Tétouan, Morocco
Departament de Química Inorgànica and Institut de Recerca de Química Teòrica i Computacional (IQTC), Universitat de Barcelona, Av. Diagonal 647, Barcelona, Spain
Institució Catalana de Recerca i Estudis Avançats (ICREA) and Instituto de Ciencia Molecular (ICMol), Universitat de València, Paterna, València, Spain
Laboratory of Inorganic Chemistry, Department of Chemistry, University of Jyväskylä, Jyväskylä, Finland
The reaction of Kpymca (pymca = pyrimidine-2-carboxylato anion) with MX2·6H2O and tmda (N,N,N′,N′-tetramethylethylenediamine) in 1 : 3 : 3 molar ratio, using a MeOH/water mixture (3 : 1) as solvent, afforded the hexanuclear complexes [M6(u-pymca)6(tmda)6]X6·4H2O (M = NiII, X = ClO4-1, BF4-2; M = CoII, X = ClO4-3). The reaction of pymca with either Cu(ClO4)2·6H2O or Cu(BF4)2·6H2O did not lead to any definite product. However, in the presence of strong coordinating chloride anions the linear tetranuclear complex [Cu4(u-pymca)3Cl(H2O)](ClO4)4·4.5H2O 4 could be obtained. The structures of 1–3 are very similar and consist of wheel-shaped hexanuclear [M6(u-pymca)6(tmda)6]6+ cations, with pseudo-D3d symmetry in which the ligand acts in a bis(chelating)/bridging mode. The pyrimidine rings of the ligands converge alternatively above and below the plane of the wheel toward the normal to this plane, leading to the formation of a bowl-shaped capsule, which is occupied by one ClO4- (1 and 3) or BF4- (2) anion. There exist tight contacts between ClO4-/BF4- and the π-electron density of the pyrimidine rings of the ligands. The tetranuclear cations of 4 exhibit a zig-zag linear conformation, in which copper ions are bridged by three bis(chelating)/bridging pymca ligands. Variable-temperature magnetic susceptibility studies reveal that complexes 1 and 4 show moderate antiferromagnetic coupling between the metal ions through the pymca ligands with J = -26.3 cm-1 for 1, and J1 = -16.3 cm-1 and J2 = -43.78 cm-1 for 4. The tetranuclear complex 4 has two different magnetic coupling constants accounting for the external–central (J1) and central–central (J2) copper interactions. The magnitude of the J1 and J2 values for 4 has been discussed on the basis of the geometrical factors affecting the magnetic pathways. Moreover, DFT calculations have been performed to support the relative magnitude of the J parameters in 4. A model accounting for spin–orbit coupling (λ), orbital reduction factors (Ak), axial zero-field splitting (Δ) and magnetic exchange coupling (J) was used to analyse the magnetic data of 3. The values of these parameters after the diagonalisation process were: Ak = 1.15, λ = -122 cm-1, Δ = 650 cm-1 and J = -5.2 cm-1.
This article is part of the themed collection:
The article was
received on 31 Mar 2009,
accepted on 26 May 2009
first published on 09 Jun 2009
Article type:
CrystEngComm, 2009,11,
ReferenceManager
E. Colacio, H. Aouryaghal, A. J. Mota, J. Cano, R. Sillanpää and A. Rodríguez-Diéguez,
CrystEngComm, 2009,&11, 2054
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