Single-crystals of the layered copper hydroxide acetate Cu-2(OH)(3)(CH3COO)center dot H2O were synthesized by heating copper acetate solution at 60 degrees C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X-ray diffraction, high temperature powder X-ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single-crystal X-ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite-type layered structure, space group P2(1), with the lattice parameters a = 5.5776(3) angstrom, b = 6.0733(2) angstrom, c = 18.5134(8) angstrom, beta = 91.802(4)degrees and a = 5.5875(4) angstrom, b = 6.0987(4) angstrom, c = 18.6801(10) angstrom, beta = 91.934(5)degrees for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge-sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn-Teller effect. (C) 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim