The water-insoluble title compound, catena-poly[palladium(II)-di-mu-acetato-kappa4O:O'], [Pd(C2H3O2)2]n, was obtained from a nitratopalladium solution and acetic acid as a pale-pink powder. Ab initio crystal structure determination was carried out using X-ray powder diffraction techniques. Patterson and Fourier syntheses were used for atom location and the Rietveld technique was applied for the final structure refinement. The structure consists of palladium acetate complexes connected into polymeric chains running along b, in which two Pd atoms are bridged by two acetate groups that are in a cis configuration with respect to one another. The unique Pd atom lies on a site with 2/m symmetry and the acetate moieties have imposed m symmetry; these are joined into infinite chains running along the b direction. The shortest Pd...Pd distance in the row is 2.9192 (1) A. The planes of adjacent palladium complexes are inclined towards each other, the angle between the planes being approximately 30 degrees.
The water-insoluble title compound, octakis(mu-acetato-kappa2O:O)octakis(mu-nitroso-kappa2N:O)octapalladium(II), [Pd8(CH3COO)8(NO)8], was precipitated as a yellow powder from a solution of palladium nitrate in nitric acid by adding acetic acid. Ab initio crystal structure determination was carried out using X-ray powder diffraction techniques. Patterson and Fourier syntheses were used for atom locations, and the Rietveld technique was used for the final structure refinement. The crystal structure is of a molecular type. The skeleton of the [Pd8(CH3COO)8(NO)8] molecule is constructed as a tetragonal prism with Pd atoms at the vertices. The eight NO- groups are in bridging positions along the horizontal edges of the prism. The N and O atoms of each nitroso group coordinate two different Pd atoms. The vertical edges present PdPd contacts with a short distance of 2.865 (1) A. These Pd atoms are bridged by a pair of acetate groups in a cis orientation with respect to each other. The complex has crystallographically imposed 4/m symmetry; all C atoms of the acetate groups are on mirror planes. The unique Pd atom lies in a general position and has square-planar coordination, consisting of three O and one N atom.
Seven new phases containing hexachloroplatinate [PtCl 6 ]2− and trans-1,2-dl-diammoniumcyclohexane 1,2-C 6 H 10 (NH 3 ) 2 2+ ions were obtained by crystallization from solutions with minor variation of synthesis conditions. The compounds can be applied as precursors for the synthesis of effective anticancer drug tetraplatin ([PtC 6 H 10 (NH 2 ) 2 Cl 4 ]). The phase diversity was achieved by alterations including solvent acidity, crystallization rate, temperature, type of solvent, and the reagents ratio. The compounds were characterized by chemical and thermal analysis, IR, and 1 H NMR spectroscopy. Crystal structures of the five compounds were determined by X-ray powder diffraction technique. The phases have ionic structures involving H 2 O, HCl molecules, or Cl − ions as supplementary species in the lattices. It helps to arrange some frames additionally interconnected by hydrogen bonds between ions and solvent molecules. It was suggested that crystal lattices adapted associated particles presented in solutions. It results in observed variety of the crystal structures. Besides the basic interest the obtained results are important for tetraplatin synthesis control.
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