Theoretical Prediction of the Electronic Properties of Bidentate Ligands (HEP2) and Synthesis of Bis(N-heterocyclic carbene) Silver and Palladium Complexes

A theoretical approach based on density functional theory (DFT) was developed to determine the electronic Huynh parameter for bidentate ligands (HEP2). The 13C chemical shift of the carbene carbon atom in the 1,3-diisopropylbenzimidazolin-2-ylidene ligand (iPr2-bimy) was calculated within the model...

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Detalles Bibliográficos
Autores: Carrasco-Carrasco, Carlos Jesús, Montilla, Francisco, Álvarez, Eleuterio, Galindo, Agustín
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2025
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/404838
Acceso en línea:http://hdl.handle.net/10261/404838
https://api.elsevier.com/content/abstract/scopus_id/105012639964
Access Level:acceso abierto
Palabra clave:Carbene compounds
Ligands
Nuclear magnetic resonance spectroscopy
Precursors
Silver
Inorganic chemistry
Crystallography
Descripción
Sumario:A theoretical approach based on density functional theory (DFT) was developed to determine the electronic Huynh parameter for bidentate ligands (HEP2). The 13C chemical shift of the carbene carbon atom in the 1,3-diisopropylbenzimidazolin-2-ylidene ligand (iPr2-bimy) was calculated within the model complexes [PdBr(L2)(iPr2-bimy)]+, where L2 represents a bidentate ligand. Strong correlations were observed between the calculated and experimental chemical shifts for both N-donor and C-donor L2 ligands, with R2 values of 0.9699 and 0.9926, respectively. This DFT approach demonstrates the potential for estimating the HEP2 parameter of bidentate ligands of these types. This method was applied to estimate the HEP2 values for three bis(N-heterocyclic carbene) ligands containing carboxylate groups, (diNHCR)2-, which are explored as ligands in this study. These NHC ligands were derived from three precursor compounds: 1-(carboxymethyl)-3-((3-(carboxymethyl)-1H-imidazol-3-ium-1-yl)methyl)-1H-imidazol-3-ium bromide (1a), 1-(1-carboxyethyl)-3-((3-(1-carboxyethyl)-1H-imidazol-3-ium-1-yl) methyl)-1H-imidazol-3-ium bromide (1b), and 2-(1-(2-(1-(carboxymethyl)-1H-imidazol-3-ium-3-yl)ethyl)-1H-imidazol-3-ium-3-yl)acetate bromide (1c). They were synthesized and characterized using IR, NMR, and single-crystal X-ray crystallography (for 1a and 1c). The interaction of 1a and 1c with Ag2O in the presence of aqueous sodium hydroxide produced the complexes [Na2(H2O)8][Ag2(diCH2NHCH)2] (2a) and [Na2(H2O)8][Ag2(diC2H4NHCH)2] (2c), respectively. Complex 2a was structurally characterized, revealing a binuclear structure in which the bis-carbene ligand adopts a bridging μ-κ1(C),κ1(C') coordination. Furthermore, 2a exhibited reactivity in transmetalation, allowing the synthesis of complex [Na2(H2O)10][Pd(diCH2NHCH)2] (3a) through a reaction with palladium acetate. Complex 3a, which was also structurally characterized, consists of a mononuclear tetracarbene species where each bis-carbene ligand coordinates in a bidentate κ2(C,C') fashion.