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Divergent Solution and Solid-State Structures of Mono- and Dinuclear Nickel(II) Pyridone Complexes
Organometallics ( IF 3.804 ) Pub Date : 2020-02-25 , DOI: 10.1021/acs.organomet.9b00799
Sean T. Goralski; Taylor A. Manes; Simone E. A. Lumsden; Vincent M. Lynch; Michael J. Rose

The chelating 2-pyridone ligand (E)-6-(1-((2-(methylthio)phenyl)imino)ethyl)pyridin-2(1H)-one (1) has been used to synthesize five nickel(II) complexes that have been characterized by single-crystal X-ray diffraction, UV/vis and IR spectroscopies, and benchtop magnetometry. Reaction of NiX2 (X = BF4, Cl) with 1 yielded the C2-symmetric halide-bridged Ni dimers [(μ-F)Ni2(κN,N,O-1)2N,N-1)2](BF4) (2) and [(μ-Cl)Ni2N,N,O-1)2N,N-1)(κN,N-1)] (3), where 2 is formed via a rare example of fluoride abstraction from BF4 by a transition metal. Remarkably, the reaction of Ni(OAc)2 with 1 followed by different methods of crystallization yielded three different products: the dimer [(μ-OH2)Ni2N,N,O-1)(κN,N-1)(κN,N-1)(OAc)2] (4), as well as the monomers [Ni(κN,N-1)2(MeOH)2] (5) and [Ni(κN,N-1)(κN,N-1)(OAc)(OH2)] (6). This observation is emblematic of the soft energy landscape of coordination motifs and nuclearity that pyridone ligands provide with late 3d transition metals. To better understand the solution versus solid-state speciation, solid-state UV/vis reflectance and solution-state UV/vis absorbance spectra were obtained. Surprisingly, the solution-state UV/vis spectra of 4 and 6 each provided nearly identical absorption spectra (λmax ≈ 360 nm), which matched neither of the solid-state reflectance spectra of 4 or 6 (λ ≈ 590, 790, 970 nm; 3A2g3T1g, 3A2g→1E2g, and 3A2g3T2g, respectively). Rather, the solution spectra are consistent only with the spectroscopic features (MLCT) of a conventional square-planar Ni(II) species.
更新日期:2020-02-25

 

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