Bmim cl

General aspects. All reactions and sample handling were carried out under a dried argon atmosphere using standard Schlenk techniques or gloveboxes. Reactions were performed in Schlenk flasks and glass ampoules that were evacuated ( p < 10 -3 mbar), heated and flashed with argon three times prior to use. The starting materials PbCl 2 (99.99%, ABCR), Mn 2 (CO) 10 (99%, ABCR) and AlCl 3 (99.99%, Sigma-Aldrich) were used as received. [BMIm]Cl (99%, Iolitec) was dried under reduced pressure (10 -3 mbar) at 130 °C for 48 h. All compounds were handled and stored in argon-filled gloveboxes (MBraun Unilab, c(O 2 , H 2 O) < 0.1 ppm).
[Pb{Mn(CO) 5 } 3 ][AlCl 4 ]. 40 mg (0.144 mmol, 1 eq.) of PbCl 2 , 96.5 mg (0.288 mmol, 2 eq.) of Mn 2 (CO) 10 , 500 mg (2.863 mmol) of [BMIm]Cl and 381.8 mg (2.863 mmol) of AlCl 3 were heated under argon in a sealed glass ampoule for 96 h at 130 °C. After cooling to room temperature with a rate of 1 K h -1 , the title compound was obtained as dark red crystals together with blue needles of [Mn(CO) 6 ][AlCl 4 ] as a minor phase. [Pb{Mn(CO) 5 } 3 ][AlCl 4 ] is highly sensitive to air and moisture and needs to be handled under inert conditions. Since the title compound could not be obtained phase-pure, the crystals for characterization were manually separated by crystal picking.