Abstract
Treatment of anhydrous CuCl 2 with excess NMe 3 at room temperature gives the yellow mono-adduct CuCl 2·1.1NMe 3 ( I). Attempted recrystallization of I from CH 2Cl 2 provides the orange tetrachlorocuprate(II) salt [Me 3NCH 2Cl] 2[CuCl 4] ( II). The same product is obtained from direct treatment of CuCl 2 with a mixture of NMe 3/CH 2Cl 2. The structure of II has been determined by conventional X-ray diffraction techniques: crystals are monoclinic, space group P2 1/n with cell constants a=17.20(1), b=11.78(1), c=9.067(7) Å, β=90.5(1)°, U=1837.0 Å 3, Z=4. The final R value for 1620 unique reflections ( I> 2σ( I)) is 0.062 ( R w=0.064). The structure consists of two independent [Me 3NCH 2Cl] + cations and one discrete [CuCl 4] 2− anion whose geometry is intermediate between tetrahedral and square planar with trans ClCuCl angles of 132.5(1) and 134.4(1)° and CuCl distances in the range 2.232(3)–2.253(3) Å.
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