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Synthesis, Crystal Structure and Thermal Behavior of Gadolinium Dicyanamide Dihydrate Gd[N(CN) 2 ] 3 · 2 H 2 O
Author(s) -
Nag Abanti,
Schnick Wolfgang
Publication year - 2006
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200500479
Subject(s) - dicyanamide , crystallography , crystal structure , chemistry , square antiprism , gadolinium , ion , molecule , aqueous solution , rietveld refinement , lanthanide , ionic liquid , biochemistry , organic chemistry , catalysis
Gadolinium dicyanamide dihydrate Gd[N(CN) 2 ] 3 · 2 H 2 O was prepared by ion exchange in aqueous solution followed by evaporation of the solvent at room temperature. Gd[N(CN) 2 ] 3 · 2 H 2 O was characterized by single‐crystal structure analysis, FTIR spectroscopy and DSC analysis. In the crystal there are three crystallographically independent [N(CN) 2 ] − ions and Gd 3+ which are coordinated by six N atoms from six different [N(CN) 2 ] − ions and two O atoms from two water molecules forming an irregular quadratic antiprism. Four H bonds have been identified in the structure of Gd[N(CN) 2 ] 3 · 2 H 2 O, two of them running to terminal N atoms and two to the bridging N atoms of dicyanamide ions (Gd[N(CN) 2 ] 3 · 2 H 2 O: P 2 1 / n (no. 14), a = 7.4845(15) Å, b = 11.529(2) Å, c = 13.941(3) Å, β = 93.98(3)°, Z = 4, 1948 reflections, 175 parameters, R 1 = 0.0493). The DSC analysis indicates that Gd[N(CN) 2 ] 3 · 2 H 2 O looses the crystal water at temperatures around 130 – 140 °C forming anhydrous Gd[N(CN) 2 ] 3 , the structure of which has been refined by the Rietveld method based on X‐ray powder diffraction data. Gd[N(CN) 2 ] 3 was found to be isotypic with Ln[N(CN) 2 ] 3 (Ln = La, Ce, Pr, Nd, Sm and Eu) which previously have been described in the literature.