Abstract
The crystal structure of [Cu(phen)2(O2CMe)][ClO4]·2H2O (1), [Cu(phen)2(O2CMe)][NO3]·2H2O (2), and [Zn(phen)2(O2(CMe)][BF4]·2H2O (3) have been determined by X-ray analysis. Complex (1) crystallises in the monoclinic space group P2/c with a= 9.671(3), b= 8.282(3), c= 17.595(4)A, β= 109.63(2)°, and Z= 2; (2) crystallises in the triclinic space group P with a= 14.728(2), b= 10.499(2), c= 8.603(2)A, α= 104.19(5), β= 83.97(5), γ= 96.81(5)°, and Z= 2;(3) crystallises in the monoclinic space group P2/c with a= 9.659(2), b= 8.262(2), c= 17.651(2)A, β= 109.06(5)°, and Z= 2. The MN4O2 chromophore in all three complexes has a cis-octahedral stereochemistry. In (1) and (3) the metal atoms have C2 symmetry and in (1) there is a marked cis distortion of the Cu–O distances. In (2) a distortion of the CuN4O2 chromophore towards a square pyramidal (4 + 1 + 1*) stereochemistry is present. The polycrystalline e.s.r. spectra of (1) and (2) and of 10% copper(II)-doped (3) are temperature variable, consistent with a fluxional CuN4O2 chromophore stereochemistry. The temperature variability of the single-crystal e.s.r. spectra of (1), (2), and copper(II)-doped (3) is restricted to the CuN2O2 plane, consistent with two-dimensional fluxional behaviour. The electronic reflectance spectra of (1) and (2) involve two peaks at ca. 10 000 and ca. 14 000 cm–1 and relate to the underlying static CuN4O2(4 + 1 + 1*) chromophore stereochemistry.
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