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About alkali metal dicyanamides: syntheses, single-crystal structure determination, DSC/TG and vibrational spectra of KCs[N(CN)₂]₂ and NaRb₂[N(CN)₂]₃ · H₂O

Author:
Reckeweg, Olaf, Wakabayashi, Ryo H., DiSalvo, Francis J., Schulz, Armin, Schneck, Christof, Schleid, Thomas
Source:
Zeitschrift für Naturforschung 2015 v.70 no.6 pp. 365-372
ISSN:
1865-7117
Subject:
X-ray diffraction, aqueous solutions, crystals, differential scanning calorimetry, ethanol, evaporation, mixing, sodium, solvents, thermogravimetry
Abstract:
Transparent colorless crystals of KCs[N(CN)₂]₂ and NaRb₂[N(CN)₂]₃ · H₂O were obtained by blending aqueous solutions of Na[N(CN)₂] and RbF or KF, respectively. After evaporation of the water, the remaining solid was extracted with absolute ethanol and the solvent was allowed to evaporate at r. t.. KCs[N(CN)₂]₂ crystallizes in the space group C2/c (no. 15) with the cell parameters a = 1382.7(2), b = 998.1(1) and c = 1455.4(2) pm, and β = 118.085(4) °. The structure of NaRb₂[N(CN)₂]₃ · H₂O is exhibiting the space group P6₃/m (no. 176) with the cell parameters a = 705.98(7) and c = 1462.89(12) pm. Single-crystalline α-K[N(CN)₂] was obtained while attempting to synthesize ‘NaK₂[N(CN)₂]₃’, corroborating the results of previous X-ray powder diffraction experiments. Vibrational spectra and DSC/TGA analyses complete our results.
Agid:
5224982