Synthesis and Crystal Structure of Tris[2-(2-imidazolinyl)phenolato]ruthenium(III)

Ryoji MITSUHASHI, Masahiro MIKURIYA
2020 X-ray Structure Analysis Online  
2-(2-Imidazolinyl)phenolate (Himn -) is a versatile bidentate ligand that forms unique supramolecular hydrogen-bonded networks. Owing to the formation of the supramolecular structures, transition-metal complexes with Himnexhibit interesting properties. For instance, [Co III (Himn)3] shows a mer/fac geometrical interconversion upon crystallization. 1 Furthermore, [Co3(Himn)6]Cl2 and [Co II (Himn)2] exhibit a single-molecule magnet behavior. In [Co3(Himn)6]Cl2, the formation of a trigonal
more » ... a trigonal hydrogen-bond sheet structure imposes the coordination geometry of the Co II ion in an ideal D3d symmetry to enhance the magnetic anisotropy. 2 In [Co II (Himn)2], the formation of a 1-dimensional hydrogen-bond chain structure is crucial for zero-field slow magnetic relaxation. 3 To extend our study on this ligand system to 4d metal ions, we synthesized and crystallographically characterized a mononuclear analogue of Himncomplex with a ruthenium(III) center, [Ru(Himn)3]•DMF (Fig. 1 , DMF = N,N-dimethylformamide). The ligand precursor, 2-(2-imidazolinyl)phenol (H2imn), was synthesized by a previously reported procedure. 4 The title compound was prepared by a reaction of RuCl3•nH2O and Himnin a 1:3 ratio. A 20-mL ethanol solution of RuCl3•nH2O (42.1 mg), H2imn (96.7 mg) and triethylamine (80 μL) was refluxed for 6 h. After cooling the reaction mixture to room temperature, red precipitate was collected by filtration. The precipitate was dried under vacuum over P2O5. Yield: 65.1 mg (50%). An X-ray-quality crystal was obtained by a layer diffusion of DMF solution to acetonitrile. The crystal data are included in Table 1 . X-ray crystallographic data were collected on a Bruker smart APEX CCD diffractometer at 90(2)K. The integrated and scaled data were empirically corrected with SADABS. 5 The initial structure was solved by
doi:10.2116/xraystruct.36.33 fatcat:bapvd6dygzgdncoo47pfh3w4ba