3 years ago

Metal-Thiobenzoato Complexes: Synthesis, Structure and Processing as Carbon Supported Nanoparticles

Pascual Roman, Daniel Vallejo-Sánchez, Monica Lanchas, Antonio Luque, Sonia Pérez-Yáñez, Oscar Castillo, Garikoitz Beobide
Six new compounds of formula [M(TBn)2L] [TBn: thiobenzoato; M: Pd(II), Zn(II), Cd(II); L: 2,2'-bipyridine (bpy), 1,10-phenanthroline (phen), 1,2-di-(4-pyridil)-ethylene (bpe), neocuproine (neo), adenine (ade)] were obtained by the reaction of M(CH3COO)2·2H2O with thiobenzoic acid and N-heterocyclic ligands. The use of chelating ligands and adenine led to monomeric compounds: [Pd(TBn)2(bpy)] (PdBPY), [Pd(TBn)2(phen)] (PdPHEN), [Zn(TBn)2(neo)] (ZnNEO), [Cd(TBn)2(neo)] (CdNEO), and [Cd(TBn)2(ade)(CH3OH)] (CdADE). In these compounds the metal is bonded to sulfur atoms of two Tbn anions while the remaining coordination positions are completed by the donor atoms of the ancillary ligands. The bridging capability of the bpe ligand gave rise to the polymeric [Cd(TBn)2(μ-bpe)]n (CdBPE) compound. The presence of direct sulfur-metal bonds and carbon rich co-ligands enabled these complexes to yield by means of a dry thermolysis process a set of metallic and metal sulfide nanoparticles embedded into a carbonaceous support. The process to produce the latter materials consisted in an aerobic thermolysis using moderate temperatures (300-500ºC) and short exposure times (minute scale). The analysis of the XRD patterns and SEM/TEM images reveal that the carbonaceous matrix hosts well dispersed nanocrystallites. The influence of the M(II) atom, ancillary ligand and thermal treatment parameters on the crystalline phase, size and purity of the resulting carbon supported nanoparticles is discussed.

Publisher URL: http://onlinelibrary.wiley.com/resolve/doi

DOI: 10.1002/ejic.201701475

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