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Título: | Lithium Di-‐ and Trimethyl Dimolybdenum(II) Complexes with Mo-‐Mo Quadruple Bonds and Bridging Methyl Groups |
Autor: | Curado, Natalia CSIC ORCID; Carrasco, Mario CSIC; Álvarez, Eleuterio CSIC ORCID ; Maya, Celia CSIC ORCID; Peloso, Riccardo CSIC ORCID; Rodríguez, Amor CSIC ORCID; López-Serrano, Joaquín CSIC ORCID CVN; Carmona, Ernesto CSIC ORCID | Palabras clave: | Bridging methyl groups Multiple bonds Molybdenum NMR spectroscopy Competitional studies |
Fecha de publicación: | 2015 | Editor: | American Chemical Society | Citación: | Journal of the American Chemical Society, 137 (38), pp 12378–12387 (2015) | Resumen: | New dimolybdenum complexes of composition [Mo2{μ-Me}2Li(S)}(μ- X)(μ-N^N)2] (3a−3c), where S = THF or Et2O and N^N represents a bidentate aminopyridinate or amidinate ligand that bridges the quadruply bonded molybdenum atoms, were prepared from the reaction of the appropriate [Mo2{μ-O2CMe}2(μ-N^N)2] precursors and LiMe. For complex 3a, X = MeCO2, while in 3b and 3c, X = Me. Solution NMR studies in C6D6 solvent support formulation of the complexes as contact ion pairs with weak agostic Mo−CH3···Li interactions, which were also evidenced by X-ray crystallography in the solid-state structures of the molecules of 3a and 3b. Samples of 3c enriched in 13C (99%) at the metal-bonded methyl sites were also prepared and investigated by NMR spectroscopy employing C6D6 and THF-d8 solvents. Crystallization of 3c from toluene:tetrahydrofuran mixtures provided single crystals of the solvent separated ion pair complex [Li(THF)4] [Mo2(Me)2(μ-Me){μ-HC(NDipp)2}2] (4c), where Dipp stands for 2,6-iPr2C6H3. A computational analysis of the Mo2(μ-Me)2Li core of complexes 3a and 3b has been developed, which is consistent with a small but non-negligible electron-density sharing between the C and Li atoms of the mainly ionic CH3···Li interactions. | Versión del editor: | http://dx.doi.org/10.1021/jacs.5b07899 | URI: | http://hdl.handle.net/10261/123628 | DOI: | 10.1021/jacs.5b07899 |
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