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Zeitschriftenartikel:

M. C. Aragoni, V. Lippolis, G. Kickelbick, A. Moghimi:
"A Novel Proton Transfer Self-Associated Compound Containing Dipicolinic Acid and Guanidine and its Cd(??)Complex: Synthesis, Characterization, Crystal Structure, and Solution Studies";
Zeitschrift für Anorganische und Allgemeine Chemie, 630 (2004), S. 617 - 624.



Kurzfassung englisch:
A novel 1:2 proton transfer self-assocd. compd. LH2, (CG+)2(pydc2-), was synthesized from the reaction of dipicolinic acid, pydcH2, (2,6-pyridinedicarboxylic acid), and guanidine hydrochloride, (GH+)(Cl-). The characterization was performed using IR, 1H and 13C NMR spectroscopy and single-crystal x-ray diffraction. LH2◊H2O crystallizes in the space group C2/c of the monoclinic system and contains eight mols. per unit cell. The unit cell dimensions are: a 26.480(5), b 8.055(2), c 14.068(3) .ANG.. The 1st coordination complex (GH)2[Cd(pydc)2]◊2H2O, was prepd. using LH2 and Cd(II) iodide, and characterized by 1H and 13C NMR spectroscopy and x-ray crystallog. The crystal system is triclinic with space group P.hivin.1 with one mol. per unit cell. The unit cell dimensions are: a 8.5125(7), b 11.0731(8), c 13.2404(10) .ANG.. The Cd(II) atom is six-coordinated with a distorted octahedral geometry. The two pydc2- units are almost perpendicular to each other. The protonation consts. of the building blocks of the pydc-guanidine adduct, the equil. consts. for the reaction of pydc2- with guanidine and the stoichiometry and stability of the Cd2+ complex with LH2 in aq. soln. were accomplished by potentiometric pH titrn. The soln. studies strongly support a self-assocn. between pydc2- and GH+ with a stoichiometry for the CdII complex similar to that obsd. for the isolated cryst. complex. In fact, the [Cd(pydc)2]2- complex is the most abundant species in soln. (>90%) at a pH > 5.


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