resumo
The synthesis and characterization of the multicomponent crystal formed by salicylic acid and 1,2-phenylenediamine (a diarylamine) are reported. The crystals are in the salt rather than cocrystal form, as witnessed by X-ray photoelectron spectroscopy, solid-state NMR, and infrared spectroscopy. H-1 double-quantum-single-quantum NMR was pivotal in confirming the proton transfer from the salicylic acid to the amine group of the basic coformer 1,2-phenylenediamine. DFT calculations were used for the geometry optimization of the hydrogen atom positions, and for calculating the NMR chemical shifts of the two possible salt/cocrystal X-ray diffraction models.
palavras-chave
SOLID-STATE; X-RAY; SUPRAMOLECULAR HETEROSYNTHONS; 1-1 COMPLEX; CO-CRYSTAL; COCRYSTAL; SALT; SOLUBILITY; CRYSTALLOGRAPHY; IDENTIFICATION
categoria
Chemistry; Crystallography
autores
Tier, AZ; Wust, KM; Vieira, JCB; Sardo, M; Cendak, T; Mafra, L; Rocha, J; Gindri, IM; Horner, M; Frizzo, CP
nossos autores
João Rocha
Prof. Catedrático
Luís Mafra
Investigador Principalagradecimentos
The authors are thankful for the financial support from the National Council of Scientific and Technological Development (Conselho Nacional de Desenvolvimento Cientifico e Tecnologico-CNPq -Grant No. 432201/2018-1. and from the Rio Grande do Sul State Foundation for Research Support (Fundacao de Amparo a Pesquisa do Estado do Rio Grande do Sul-FAPERGS)-Grant No. 17/2551-0000 944-4. This study was financed in part by the Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior -Brasil (CAPES) -Finance Code 001. The fellowships from CNPq (C. P. F., and M. H.) and CAPES (A. Z. T, J. C. B. V. and K. M. W.) are also acknowledged. This work was also developed as part of Project CICECO-Aveiro Institute of Materials (FCT Ref. UID/CTM/50011/2019), financed by national funds through the FCT/MCTES. We are also grateful to the Portuguese NMR Network (RNRMN) and Roteiro Nacional de Infraestruturas (Project PTNMR 22161).