Synthesis and characterization of new trimeric rhenium(I) complexes. The influence of steric factors on the size of pyrazolonaterhenium(I) metallomacrocycles.
The reaction of [ReX(CO)5] with thiosemicarbazones H2L(R) derived from beta-keto esters (X = Cl, Br; R = Me, Ph) allowed the isolation of cyclic trimeric complexes [Re3(pyz(R))3(CO)9], where pyz(R) is the pyrazolonate corresponding to the thiosemicarbazone. Electron spray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS) monitoring of the reactions of H2L(Ph) in toluene confirmed that the trimer was formed in the reaction mixture and no higher oligomer was detected. These studies, together with the X-ray structures of the trimeric complexes, afford new insight into the factors influencing the self-assembly of pyrazolonaterhenium(I) complexes.
Barbazán
Paula
P
Departamento de Química Inorganica, Facultade de Química, Edificio de Ciencias Experimentais, Universidade de Vigo, E-36310 Vigo, Galicia, Spain.
Carballo
Rosa
R
Casas
José S
JS
García-Martínez
Emilia
E
Pereiras-Gabián
Gumersindo
G
Sánchez
Agustín
A
Vázquez-López
Ezequiel M
EM
D018360:Crystallography, X-Ray; D008024:Ligands; D047028:Macrocyclic Compounds / Q000138:chemical synthesis / Q000737:chemistry; D008958:Models, Molecular; D015394:Molecular Structure; D009942:Organometallic Compounds / Q000138:chemical synthesis / Q000737:chemistry; D047069:Pyrazolones / Q000737:chemistry*; D012211:Rhenium / Q000737:chemistry*; D013237:Stereoisomerism
D008024:Ligands; D047028:Macrocyclic Compounds; D009942:Organometallic Compounds; D047069:Pyrazolones; D012211:Rhenium