A B C
Z. Naturforsch. 2014, 69b, 277 – 288
doi:10.5560/ZNB.2014-3272
Structural Diversity of Hydrogen-Bonded Networks of [Co(NH3)6]3+ Complex Cations and Acetylenedicarboxylic Acid Anions
Rüdiger W. Seidel1, Richard Goddard1, Verena Gramm2, and Uwe Ruschewitz2
1 Max-Planck-Institut für Kohlenforschung, Kaiser-Wilhelm-Platz 1, 45470 Mülheim an der Ruhr, Germany
2 Department für Chemie der Universität zu Köln, Greinstraße 6, 50939 Köln, Germany
Reprint requests to Dr. Rüdiger W. Seidel and Prof. Dr. Uwe Ruschewitz. Fax: +49(0)208 306 2989; +49(0)221 470 3285. E-mail: Ruediger.Seidel@rub.de; E-mail: Uwe.Ruschewitz@uni-koeln.de
Received October 6, 2013 / published online March 17, 2014
The crystal structure of [Co(NH3)6](ADC)(HADC) · 2 H2O (1) (ADC2− = acetylenedicarboxylate) (P21/n, Z = 4) was mistakenly described as containing the [Co(H2O)6]3+ ion [I. Stein, U. Ruschewitz, Z. Naturforsch. 2011, 66b, 471–478]. A revision is reported. While attempting to reproduce 1, we isolated phase-pure crystalline material of [Co(NH3)6]Cl2(HADC) · H2O (2), the crystal structure of which was also reported in the article above. Upon standing in the aqueous mother liquor at room temperature for several days, the needle-shaped crystals of 2 disappear, while block-shaped crystals of the formerly unknown compound [Co(NH3)6](ADC)(HADC) (3) grow. Satellite peaks in the X-ray diffraction frames indicate that the crystal structure is incommensurately modulated. Dissolving crystals of 3 in water at elevated temperature leads to plate-shaped crystals of the new compound [Co(NH3)6]2(ADC)3 · 3 H2O (4) upon slow cooling to room temperature. Compounds 24 were investigated by elemental analysis, powder X-ray diffraction and infrared spectroscopy. Structural characterization of 4 by single-crystal X-ray analysis was also achieved (P1̅, Z = 2). Complex 1, however, could not be reproduced.
Key words: Acetylenedicarboxylic Acid, Cobalt, Coordination Compound, Crystal Structure, Hydrogen Bonding
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