Stabilization of molecular LiF and LiFHF inside metallamacrocyclic hosts |
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Authors: | Lehaire Marie-Line Scopelliti Rosario Severin Kay |
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Institution: | Institut de Chimie Moléculaire et Biologique, Ecole Polytechnique Fédérale de Lausanne, 1015 Lausanne, Switzerland. |
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Abstract: | Complexes of molecular LiF and LiFHF were synthesized using the metallamacrocyclic receptors (cymene)Ru(C(5)H(3)NO(2))](3) (1), CpRh(C(5)H(3)NO(2))](3) (2), and CpIr(C(5)H(3)NO(2))](3) (3). LiBF(4) complexes of 1-3 were prepared and subsequently treated with F(-) or FHF(-) to give the desired products in an anion-exchange reaction. All complexes were characterized by multinuclear NMR spectroscopy ((1)H, (13)C, (19)F, (7)Li). Strong scalar coupling between (7)Li and (19)F is observed for the LiF and the LiFHF complexes ((1)J(LiF) = 91-103 Hz). The LiFHF adduct of 1 displays fluxional behavior with fast exchange of the two fluorine atoms. The structures of the complexes 1.LiBF(4), 2.LiBF(4), 1.LiF, 2.LiF, 1.LiFHF, and 3.LiFHF were determined by single-crystal X-ray analysis. Li-F bond lengths between 1.77 and 1.81 A were found. The LiFHF complexes show a hydrogen difluoride anion coordinated in a bent fashion via one fluorine atom to the lithium ion. |
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