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Synthesis and Reduction of Heteroleptic Bis(cyclopentadienyl) Uranium(III) Complexes. | LitMetric
Heteroleptic U(III) complexes supported by bis(cyclopentadienyl) frameworks have been synthesized to examine their suitability as precursors to U(II) complexes. The newly synthesized (CMe)U(OCHBu-2,6-Me-4), (CMe)U(OCHAd-2,6-Bu-4) (Ad = 1-adamantyl), (CMe)U(CH), and (CMe)U(CMeH) are compared with (CMe)U[N(SiMe)], (CMe)U[CH(SiMe)], and (CMe)U[N(SiMe)]. An improved synthesis of (CMe)U(μ-Ph)BPh was developed, which was used to synthesize (CMe)U(CMeH). Since the X-ray crystal structure of (CMe)U(OCHBu-2,6-Me-4) contained two very different molecules in the asymmetric unit with 115.7(5)° and 166.0(5)° U-O-C angles, the (CMeH)U(OCHBu-2,6-Me-4) and (CMe)Ce(OCHBu-2,6-Me-4) analogues were synthesized and characterized by X-ray diffraction for comparison. Electrochemical studies in THF with a 100 mM [BuN][BPh] supporting electrolyte showed U(IV)/U(III) and U(III)/U(II) redox couples for all the heteroleptic complexes except (CMe)U(CH). Chemical reduction of all heteroleptic compounds formed dark blue solutions characteristic of U(II) when reacted with KC at -78 °C, but none formed isolable U(II) complexes. The targeted U(II) complexes, [(CMe)U(OCHBu-2,6-Me-4)], {(CMe)U[CH(SiMe)]}, [(CMe)U(CH)], and [(CMe)U(CMeH)], were analyzed by density functional theory, and a 5f6d electron configuration was found to be the ground state in each case.
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