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Síntese, cristalografia e atividade biológica de complexos triazenidos de Au(I), Ag(I), Pd(II) E Pt(II) / Synthesis, crystallographic and biological activity of triazenide complexes of Au(I), Ag(I), Pd(II) E Pt(II)Locatelli, Aline 24 August 2012 (has links)
Conselho Nacional de Desenvolvimento Científico e Tecnológico / This work presents the synthesis of compounds and their triazenes complexes of gold(I), silver(I), platinum(II) and paladium(II). Triazenes have three nitrogen atoms connected in sequence [ N=N N(H) ] and, when deprotonated, they become excellent ligands in coordination chemistry. The synthesized ligands have ortho nitro substituent and variable substituent halogenated, or also in a position. Characterizations were performed using various techniques: thermogravimetric analysis, ultraviolet and visible spectroscopy, infrared and proton nuclear magnetic resonance, and the main focus of this work was the structural characterization of the complexes by X-ray diffraction on monocrystal, with emphasis the study of these supramolecular arrangements. Nitro and halide substituents (F, Cl, Br and I) providing the formation of various types of interactions, which form supramolecular arrangement. Four ligands were synthesized 1-(2-flurorphenyl)-3-(2-nitrophenyl)triazene (A), 1-(2-chlorophenyl)-3-(2-nitrophenyl)triazene (B), 1-(2-bromophenyl)-3-(2-nitrophenyl)triazene (C), 1-(2-iodophenyl)-3-(2-nitrophenyl)triazene (D) and thirteen complexes
{[1-(2-fluorophenyl)-3-(2-nitrophenyl)triazenide](triphenilphosfine)gold(I)} (1), {[1-(2-chlorophenyl)-3-(2-nitrophenyl)triazenide](triphenilphosfine)gold(I)} (2), {[1-(2-bromophenyl)-3-(2-nitrophenyl)triazenide](triphenilphosfine)gold(I)} (3), {trans- bis-[1-(2-chlorophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)paladium(II)} (4), {trans- bis-[1-(2-bromophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)paladium(II)} (5), {trans- bis-[1-(2-iodophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)paladium(II)} (6), {cis- bis-[1-(2-chlorophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)platinum(II)} (7), {cis- bis-[1-(2-bromophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)platinum(II)} (8), {cis- bis-[1-(2-iodophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)platinum(II)} (9), {trans-[1-(2-bromophenyl)-3-(2-nitrophenyl)triazenide]-bis-(pyridine)(chloro)platinum(II)} (10), {cis- [1-(2-bromophenyl)-3-(2-nitrophenyl)triazenide]-ditriphenylphosfine(chloro)platinum(II)} (11), {bis-[1-(2-iodophenyl)-3-(2-nitrophenyl)triazenide]silver(I)} (12) e {[1-(2-fluorophenyl)-3-(2-nitrophenyl)triazenide](triphenylphosfine)silver(I)} (13). For the purpose of Bioinorganic studying the triazenido complexes of gold (I), and Platinum (II) were subjected to evaluation of biological activity shown promising results. / Este trabalho apresenta a síntese de compostos triazenos e seus complexos de ouro(I), prata(I), platina(II) e paládio(II). Os compostos triazenos possuem três átomos de nitrogênio ligados em sequência [ N=N N(H) ]. Quando desprotonados transformam-se em excelentes ligantes com grande exploração na química de coordenação. Os pré-ligantes sintetizados possuem substituinte nitro em posição orto e variável substituinte halogenado, também em posição orto. Foram realizadas caracterizações com diversas técnicas: análise termogravimétrica (TGA), espectroscopia ultravioleta e visível, infravermelho e ressonância magnética nuclear de próton, sendo que o foco principal deste trabalho foi a caracterização estrutural dos complexos por difração de raios-X em monocristal, com destaque no estudo supramolecular destes compostos. Os substituintes nitro e haletos (F, Cl, Br e I) proporcionam a formação de diversos tipos de interações, as quais constituem arranjo supramoleculares. Foram sintetizados quatro pré-ligante 1-(2-fluorfenil)-3-(2-nitrofenil)triazeno (A), 1-(2-clorofenil)-3-(2-nitrofenil)triazeno (B), 1-(2-bromofenil)-3-(2-nitrofenil)triazeno (C), 1-(2-iodofenil)-3-(2-nitrofenil)triazeno (D) e treze complexos
{[1-(2-fluorofenil)-3-(2-nitrofenil)triazenido](trifenilfosfina)ouro(I)} (1), {[1-(2-clorofenil)-3-(2-nitrofenil)triazenido](trifenilfosfina)ouro(I)} (2), {[1-(2-bromofenil)-3-(2-nitrofenil)triazenido](trifenilfosfina)ouro(I)} (3), {trans- bis-[1-(2-clorofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)paládio(II)} (4), {trans- bis-[1-(2-bromofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)paládio(II)} (5), {trans- bis-[1-(2-iodofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)paládio(II)} (6), {cis- bis-[1-(2-clorofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)platina(II)} (7), {cis- bis-[1-(2-bromofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)platina(II)} (8), {cis- bis-[1-(2-iodofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)platina(II)} (9), {trans-[1-(2-bromofenil)-3-(2-nitrofenil)triazenido]-bis-(piridina)(cloro)platina(II)} (10), {cis- [1-(2-bromofenil)-3-(2-nitrofenil)triazenido]-ditrifenilfosfina(cloro)platina(II)} (11), {bis-[1-(2-iodofenil)-3-(2-nitrofenil)triazenido]prata(I)} (12) e {[1-(2-fluorofenil)-3-(2-nitrofenil)triazenido](trifenilfosfina)prata(I)} (13). Para fins de estudar a Bioinorgânica dos complexos triazenidos de Ouro(I) e Platina(II), os compostos foram submetidos a avaliação de atividade biológica apresentando resultados promissores.
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