TY - JOUR
T1 - Synthesis and characterisation of palladium compounds with new polyetherpyrazole ligands
AU - Boixassa, Anna
AU - Pons, Josefina
AU - Solans, Xavier
AU - Font-Bardia, Mercè
AU - Ros, Josep
PY - 2003/3/25
Y1 - 2003/3/25
N2 - The present report is on the synthesis of new 3,5-dimethylpyrazolic derived ligands that are N1-substituted by polyether chains: 1-(2-methoxyethoxymethyl)-3,5-dimethylpyrazole (L1), 1-[2-(2-methoxyethoxymethoxy)ethyl]-3,5-dimethylpyrazole (L2) and 1-[2-[2-(2-methoxyethoxy)ethoxy]ethyl]-3,5-dimethylpyrazole (L3). These ligands form complexes with the formula [PdCl2L2] when reacting with [PdCl2(CH3CN)2] in the ratio 1M:2L. Two crystalline structures have been resolved with ligands L1 and L3, where the Pd(II) presents a square planar geometry with the ligands co-ordinated in a trans disposition. NMR studies prove the existence of two conformational diastereoisomers for each complex in solution, as a consequence of the slow rotation around the Pd-N bond: syn and anti. The reaction of ligands L1, L2 and L3 with [PdCl2(CH3CN)2] in presence of AgBF4 yields the compounds [PdClL3]BF4, characterised by elemental analysis, conductivity measurements, 1H NMR, 13C{1H} NMR, infrared spectra, and FIA ES(+)/MS. © 2002 Elsevier Science B.V. All rights reserved.
AB - The present report is on the synthesis of new 3,5-dimethylpyrazolic derived ligands that are N1-substituted by polyether chains: 1-(2-methoxyethoxymethyl)-3,5-dimethylpyrazole (L1), 1-[2-(2-methoxyethoxymethoxy)ethyl]-3,5-dimethylpyrazole (L2) and 1-[2-[2-(2-methoxyethoxy)ethoxy]ethyl]-3,5-dimethylpyrazole (L3). These ligands form complexes with the formula [PdCl2L2] when reacting with [PdCl2(CH3CN)2] in the ratio 1M:2L. Two crystalline structures have been resolved with ligands L1 and L3, where the Pd(II) presents a square planar geometry with the ligands co-ordinated in a trans disposition. NMR studies prove the existence of two conformational diastereoisomers for each complex in solution, as a consequence of the slow rotation around the Pd-N bond: syn and anti. The reaction of ligands L1, L2 and L3 with [PdCl2(CH3CN)2] in presence of AgBF4 yields the compounds [PdClL3]BF4, characterised by elemental analysis, conductivity measurements, 1H NMR, 13C{1H} NMR, infrared spectra, and FIA ES(+)/MS. © 2002 Elsevier Science B.V. All rights reserved.
KW - Crystal structures
KW - Palladium complexes
KW - Polyether ligand complexes
KW - Pyrazole complexes
U2 - 10.1016/S0020-1693(02)01384-1
DO - 10.1016/S0020-1693(02)01384-1
M3 - Article
SN - 0020-1693
VL - 346
SP - 151
EP - 157
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
ER -