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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

Síntese e Caracterização de Novos Compostos Derivados de Bis(4-Aminobenzenoselenolato) de Mercúrio(II) e Bis(4-N,N-Dimetil-aminobenzenoselenolato) de Mercúrio(II) / Synthesis and characterization of new compounds derived from Mercury(II) Bis(4-Aminobenzeneselenolate) and Mercury(II) Bis(4-N,N-Dimethyl-aminobenzeneselenolate)

Bublitz, Fabrício 18 July 2014 (has links)
Conselho Nacional de Desenvolvimento Científico e Tecnológico / This work presents the synthesis and structural analysis of the first compounds obtained through the use of the building blocks Mercury(II) bis(4-Aminobenzeneselenolate) Hg(SeC6H4NH2-4)2 and Mercury(II) bis(4-N,N-Dimethyl-Aminobenzeneselenolate) Hg(SeC6H4NMe2-4)2. Firstly, a synthetic procedure was adapted for the diaryl disselenides (4-H2NC6H4Se)2 (1a) e (4-Me2NC6H4Se)2 (1b), whose crystalline structures are been described here for the first time. From these disselenides, it were possible to obtain the mercury(II) selenolates Hg(SeC6H4NH2-4)2 (2a) e Hg(SeC6H4NMe2-4)2 (2b). By reacting 2a with mercury(II) halides and tricyclohexylphosphine, the complexes HgX(SeC6H4NH2-4)(PCy3) (3a, X = I and 3b, X = Br) and the pseudo dimer [HgCl(SeC6H4NH2-4)(PCy3)]2.2THF (4) were obtained. Instead, by reacting 2b with mercury(II) halides, the coordination polymer {[Hg2Br2(SeC6H4NMe2-4)2].DMF}n (5) and the polymeric cluster [Hg4Cl3(SeC6H4NMe2-4)5]n (6) were obtained. All the compounds with the exception of 2b were structurally determined by single crystal X-ray diffraction and 1(a-b), 2(a-b) were characterized by nuclear magnetic resonance. All the compounds were also analyzed by infrared vibrational spectroscopy and elemental analysis. / Este trabalho apresenta a síntese e análise estrutural dos primeiros compostos obtidos utilizando-se os blocos de montagem bis(4-Aminobenzenoselenolato) de Mercúrio(II) Hg(SeC6H4NH2-4)2 e bis(4-N,N-Dimetil-Aminobenzenoselenolato) de Mercúrio(II) Hg(SeC6H4NMe2-4)2. Inicialmente adaptou-se um procedimento de síntese dos disselenetos de diarila (4-H2NC6H4Se)2 (1a) e (4-Me2NC6H4Se)2 (1b), cujas estruturas cristalinas estão sendo descritas aqui pela primeira vez. A partir destes disselenetos foi possível obter os selenolatos de mercúrio(II) Hg(SeC6H4NH2-4)2 (2a) e Hg(SeC6H4NMe2-4)2 (2b). Pela reação de 2a com haletos de mercúrio(II) e tricicloexilfosfina obteve-se os complexos HgX(SeC6H4NH2-4)(PCy3) (3a, X = I e 3b, X = Br) e o pseudodímero [HgCl(SeC6H4NH2-4)(PCy3)]2.2THF (4). Já pela reação de 2b com haletos de mercúrio(II) foram obtidos o polímero de coordenação {[Hg2Br2(SeC6H4NMe2-4)2].DMF}n (5) e o cluster polimérico [Hg4Cl3(SeC6H4NMe2-4)5]n (6). Todos os compostos com exceção de 2b tiveram sua estrutura determinada por difração de raios X em monocristal e os compostos 1(a-b) e 2(a-b) foram caracterizados por ressonância magnética nuclear. Todos os compostos também foram analisados por espectroscopia vibracional na região do infravermelho e análise elementar.

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