Synthesis,characterization, and olefin polymerization of half-sandwich Ir,Rh, Ru metallacycle enclosing a nickel in the center |
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| Authors: | Ai-Quan Jia Fenglan Liu Jian-Qiang Wang Dan Liu |
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| Affiliation: | 1. Institute of Molecular Engineering and Applied Chemistry, Anhui University of Technology Ma’anshan, Anhui, PR Chinajaiquan@ahut.edu.cn;3. Institute of Molecular Engineering and Applied Chemistry, Anhui University of Technology Ma’anshan, Anhui, PR China;4. Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai, PR China |
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| Abstract: | Reactions of binuclear [Cp*Ir(μ-Cl)Cl]2 (Cp* = pentamethylcyclopentadienyl), [Cp*Rh(μ-Cl)Cl]2 and [(p-cymene)Ru(μ-Cl)Cl]2 with 2 equiv. AgOTf (OTf = O3SCF3) followed by addition of one equiv. (m-pyridyl)N=C(C10H6)C=N(m-pyridyl) (mPy-bian) linker and NiCl2·DME (DME = 1,2-dimethoxyethane) in methanol gave heterometallic cationic metallacycles [Cp*4Ir4(μ-Cl)4(μ-mPy-bian)2NiCl2](OTf)4 (1a), [Cp*4Rh4(μ-Cl)4(μ-mPy-bian)2NiCl2](OTf)4 (1b), and [(p-cymene)4Ru4(μ-Cl)4(μ-mPybian)2NiCl2](OTf)4 (1c), respectively. All the complexes are characterized by IR, NMR spectroscopy, and elemental analysis. Ni K-edge X-ray absorption spectroscopy (XAS) studies on 1a–1c reveal that nickel is six-coordinate with four nitrogens and two chlorides. Upon activation with MAO, 1a–1c showed moderate to good catalytic activity for ethylene and norbornene polymerization. |
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| Keywords: | Nickel heterometallic half-sandwich olefin polymerization metallacycles |
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