Abstract
1,3,5,7-Tetra-t-butyl-4,8-Biphenyl-1,3,5,7-tetra-aza-2,6-diplumba-4,8-diboratricyclo[4.2.0.02,5]octane-1,5-diium-2,6-diide(1)hasbeen obtained from PhB(NButLi)2 and PbCl4in hexane or from PbCl2 intetrahydrofuran and structurally characterised by X-ray diffraction.
Highlights
+ refined with a weighting scheme [ w - l = 02(F) 0.0005 F,?]
Stirring at -78°C was continued for 12 h followed by 6 h at 20 "C
In due course the solvent is removed under reduced pressure, the residue sublimed at 175"C and 0.01 mbar, and the sublimed (1) recrystallized from hexane
Summary
F Preparative details and spectroscopic datu: a solution of bis(t-butylamino)phenylborane' (0.034 mol) i n n-hexane (60 ml) was mixed with a solution (46 ml) of n-butyl-lithium (0.070 mol) in hexane at 0 "C and stirred for 12h under reflux. The suspension formed was added dropwise in the dark with stirring at -78 "C to PbC14 (0.017 mol) in pentane (200ml). Stirring at -78°C was continued for 12 h followed by 6 h at 20 "C.
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