Synthesis of a new tetra-cyanomethylated macrocyclic ligand with a nanotubular structure. X-Ray crystal structures of mono-, di-nuclear and polymeric metal complexes
González, Sonia; Valencia, Laura; Bastida, Rufina; Fenton, David E.; Macías, Alejandro; Rodríguez, Adolfo; González Sonia; Departamento de QuÃmica Inorgánica, Universidad de Santiago de Compostela; Valencia Laura; Departamento de QuÃmica Inorgánica, Universidad de Santiago de Compostela; Bastida Rufina; Departamento de QuÃmica Inorgánica, Universidad de Santiago de Compostela; Fenton David E.; Department of Chemistry, The University of Sheffield; MacÃas Alejandro; Departamento de QuÃmica Inorgánica, Universidad de Santiago de Compostela; RodrÃguez Adolfo; Departamento de QuÃmica Inorgánica, Universidad de Santiago de Compostela
Журнал:
Journal of the Chemical Society, Dalton Transactions
Дата:
2002
Аннотация:
A new pendant-armed macrocyclic ligand, L<sup>1</sup>, bearing four cyanomethyl pendant groups has been synthesized by N-alkylation of the tetraazamacrocyclic precursor L with bromoacetonitrile. The X-ray structural analysis of the ligand L<sup>1</sup> shows the formation of tubular arrays, and reveals intra- and inter-molecular Ï -stacking interactions between the pyridyl groups of the macrocyclic backbone. Metal complexes of L<sup>1</sup> have been synthesized and characterized by microanalysis, MS-FAB, conductivity measurements, IR, UV-Vis, <sup>1</sup>H and <sup>13</sup>C NMR spectroscopy and magnetic studies. Crystal structures of the ligand L<sup>1</sup> as well as of the complexes [ZnL<sup>1</sup>](NO3)2·2H2O, [Ag2L<sup>1</sup>(NO3)2] and [Ag2L<sup>1</sup>](ClO4)2·4CH3CN have been determined by single crystal X-ray crystallography. Different macrocyclic disposition has been found in relation to the metal ion employed and even when different salts of the same metal are used. The X-ray studies show the presence of two metal atoms within the macrocyclic ligand in [Ag2L<sup>1</sup>(NO3)2] and [Ag2L<sup>1</sup>](ClO4)2·4CH3CN showing a monomeric and a polymeric nature respectively. The crystal structure of [ZnL<sup>1</sup>(NO3)2]·2H2O shows a mononuclear endomacrocyclic complex with the metal ion coordinated to the six nitrogen atoms in a distorted octahedral environment.
254.4Кб