The structure of the title compound has been refined from three-dimensional X-ray diffractorneter data. Crystals are monoclinic, space group C2/c, with Z = 4 in a unit-cell of dimensions: a = 13. 1 68(2). b = 8.564(2), c = 13.858(2) 8, and = 11 7.02(1)". Full-matrix least-squares refinement, using 1280 independent reflections, has reached R 0.047. The refinement has, as expected, confirmed the original two-dimensional structure determination and much more accurate bond lengths and bond angles have been obtained : mean Cu-O(acetate) 1-969 8, Cu-O(water) 2.1 56, and Cu * * Cu is 2.61 6 8. The geometry of the acetate bridges is planar and bond lengths and angles are as expected.
The presence of a peroxocarbonate species, likely to be HC04-in pH-dependent equilibrium with C042-, in solutions of HC03-in an excess of H202 is inferred from Raman and 13C n.m.r. spectroscopy; similar evidence is presented for the presence of CO& in solutions prepared by dissolving solid peroxocarbonates (NaHC04.H20 and K2C206) in aqueous alkali.
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