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Synthesis and Characterization of Ca 2 (PO 2 NH) 4 ·8H 2 O
Author(s) -
Sedlmaier Stefan J.,
Römer S. Rebecca,
Schnick Wolfgang
Publication year - 2011
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.201100309
Subject(s) - crystallography , hydrogen bond , crystal structure , molecule , chemistry , aqueous solution , analytical chemistry (journal) , ion , crystal (programming language) , organic chemistry , chromatography , computer science , programming language
Ca 2 (PO 2 NH) 4 · 8H 2 O was obtained as single‐phase crystalline powder starting from aqueous solution of K 4 (PO 2 NH) 4 · 4H 2 O and Ca(NO 3 ) 2 · 4H 2 O. A small fiber‐like specimen has been used for single‐crystal X‐ray structure determination. In the structure of Ca 2 (PO 2 NH) 4 · 8H 2 O ( Pbcn (no. 60), a = 1700.6(3), b = 1069.3(2), c = 963.2(2) pm, Z = 4) there are (PO 2 NH) 4 4– ions in saddle conformation which are interconnected by N–H ··· O hydrogen bonds forming infinite columns running along [001]. These columns are hold together by a complex hydrogen bonding network with crystal water molecules involved. The FTIR spectrum of the title compound has been measured and the relevant bands were assigned. 31 P solid‐state NMR investigations yielded three resolved resonances with chemical shift values of –3.1, –4.9 and –7.9 ppm. DTA / TG data are also discussed.