Journal of the Chemical Society, Dalton Transactions p. 1959 - 1964 (1982)
Update date:2022-08-11
Topics:
Lappert, Michael F.
Martin, Tony R.
Raston, Colin L.
Skelton, Brian W.
White, Allan H.
A high yield sythesis of a tetrahydrofuran (thf) solution of the di-Grignard reagent (A) derived from o-bis(chloromethyl)benzene is described, as well as that of an analogue obtained from 1,2-bis(chloromethyl)-4,5-dimethylbenzene.Cooling (A) to ca. -40 deg C yields the colourless chloride-free Mg(CH2C6H4CH2-o)(thf) of unknown structure, whereas at ambient temperature a concentrated solution ( > ca. 0.1 mol dm-3) slowly (days) deposits colourless needles of <A single-crystal X-ray structure determination of the latter (R=0.054 for 1117 'observed' reflections at 295 K) shows it to be trimer.Crystals are orthorhombic, space group F2dd, with a=24.706(8), b=8.948(3), c=44.315(9) Angstroem, and Z=8; the trimeric unit lies on a crystallographic two-fold axis.Each of the three magnesiums is bridged to the other two by a -CH2C6H4CH2-o ligand, the pseudo tetrahedral co-ordination about each magnesium atom being completed by a pair of thf molecules.The utility of the di-Grignard reagent as a general metallocycle precursor is illustrated by the synthesis of
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