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Síntesis y caracterización espectroscópica, cristalográfica, térmica y morfológica de un polímero de coordinación entre cobalto y el ácido 5-(carboximetilamino)isoftálico
Synthesis and spectroscopic, crystallographic, thermal, and morphological characterization of a cobalt coordination polymer with 5-(carboxymethylamino)isophthalic acid
Síntese e caracterização espectroscópica, cristalográfica, térmica e morfológica de um polímero de coordenação entre cobalto e o ácido 5-(carboximetilamino)isoftálico
DOI:
https://doi.org/10.15446/rev.colomb.quim.v55n1.118142Palabras clave:
Ligando carboxilato, Ligando semirrígido, Ajuste Pawley (es)Carboxylate ligand, Semi-rigid ligand, Pawley refinement (en)
Ligante carboxilato, Ligante semirrígido, Refinamento de Pawley (pt)
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En este trabajo se sintetizó el ácido 5-(carboximetilamino)isoftálico (C10O6H9N) en su clorhidrato (C10O6H9N·HCl·H2O) (4) a través de una nueva ruta de síntesis que consiste en la esterificación, cianometilación e hidrólisis del ácido 5-aminoisoftálico (1). La caracterización de 4 involucró espectroscopía infrarroja por transformada de Fourier (FT-IR), resonancia magnética nuclear de hidrógeno (RMN 1H) y de carbono (RMN 13C), correlación heteronuclear vía coherencia cuántica simple (HSQC), correlación heteronuclear a múltiples enlaces (HMBC), espectrometría de masas con ionización por electro-spray (ESI-MS), análisis elemental y análisis termogravimétrico con calorimetría diferencial de barrido (TGA/DSC). A partir del compuesto 4, se sintetizó por el método hidrotermal en medio básico un nuevo polímero de coordinación (CP) con cobalto (Co): [Co2(C10O6H7N)(OH)2]⸱5H2O, llamado 1DCP-Co. La caracterización del nuevo CP se llevó a cabo mediante análisis elemental, análisis de espectroscopía de fotoelectrones de rayos X (XPS), IR, TGA/DSC y se determinó el área superficial a través de isotermas de adsorción usando el modelo Brunauer-Emmett-Teller (BET) con un valor de 2,11 m2/g. La caracterización cristalográfica se llevó a cabo mediante un indexado en el que se determinó, a través del ajuste de Pawley, que el perfil de difracción corresponde a una fase única. La investigación de estos compuestos constituye un avance en la investigación de nuevas rutas sintéticas de ligandos y materiales en la química de coordinación.
In this work, 5-(carboxymethylamino)isophthalic acid (C10O6H7N) was synthesized in its hydrochloride form (C10O6H9N·HCl·H2O (4) through a new synthesis route which consists of the esterification, cyanomethylation and hydrolysis of 5-aminoisophthalic acid (1). The characterization of 4 involved infrared spectroscopy (IR), hydrogen (1H) and carbon (13C) nuclear magnetic resonance (RMN), heteronuclear correlation via single quantum coherence (HSQC), heteronuclear correlation to multiple bonds (HMBC), electrospray ionization mass spectrometry (ESI-MS), elemental analysis, and thermogravimetric analysis with scanning calorimetry (TGA/DSC). From compound 4, a new cobalt-based coordination polymer (CP), [Co2(C10O6H7N)(OH)2]·5H2O, named 1DCP-Co, was synthesized via a hydrothermal method in basic medium. The characterization of this new coordination polymer was carried out using elemental analysis, X-ray photoelectron spectroscopy (XPS), IR, and TGA/DSC. The surface area was determined using adsorption isotherms using the Brunauer-Emmett-Teller (BET) model, yielding a value of 2.11 m2/g. Crystallographic characterization was performed by indexing, confirming that the diffraction profile corresponds to a single phase through Pawley refinement. The study of these compounds represents progress in the development of new synthetic routes for ligands and materials in coordination chemistry.
Neste trabalho, o ácido 5-(carboximetilamino)isoftálico (C10O6H9N) foi sintetizado na sua forma cloridrato (C10O6H9N·HCl·H2O) (4) por meio de uma nova rota sintética que envolve a esterificação, cianometilação e hidrólise do ácido 5-aminoisoftálico (1). A caracterização do composto 4 incluiu espectroscopia no infravermelho (IR), ressonância magnética nuclear de hidrogênio (RMN 1H) e carbono (RMN 13C), correlação heteronuclear via coerência quântica simples (HSQC), correlação heteronuclear com múltiplas ligações (HMBC), espectrometria de massa por ionização por electrospray (ESI-MS), análise elementar e análise termogravimétrica com calorimetria de varredura (TGA/DSC). A partir do composto 4, foi sintetizado, pelo método hidrotermal em meio básico, um novo polímero de coordenação (CP) com cobalto: [Co2(C10O6H7N)(OH)2]·5H2O, denominado 1DCP-Co. A caracterização desse novo CP foi realizada por análise elementar, espectroscopia de fotoelétrons excitados por raios X (XPS), IR e TGA/DSC. A área superficial foi determinada por meio de isotermas de adsorção utilizando o modelo de Brunauer-Emmett-Teller (BET), resultando em um valor de 2,11 m²/g. A caracterização cristalográfica foi realizada por indexação, e o ajuste de Pawley confirmou que o perfil de difração corresponde a uma única fase. A investigação desses compostos representa um avanço na pesquisa de novas rotas sintéticas para ligantes e materiais em química de coordenação.
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