Synthesis and structure of ammonium tricupric(II)‐octadecatungsto‐diantimonate(III)

This paper reports the synthesis, properties and structure of (NH 4 ) 12 , [Cu 3 (H 2 O) 3 (SbW 9 O 33 ) 2 ]. 11H 2 O. The compound was prepared by the depolymerization reaction of (NH 4 ) 18 [(NH 4 )Sb 9 W 21 O 86 n ‐H 2 O, which was proposed firstly as a method of preparing new heteropoly tungstoantimonate(III). Its properties were characterized by IR, Raman, UV‐VS spectra, TG‐DTA thermal analysis, and X‐ray single crystal analysis. The crystal is orthorhombic, with space group D 16 2b ‐ Pnma. The crystal data are: a = 15.423(4), b = 19.307(6), c = 30.275(6)Å, V = 9015.0Å 3 , Z = 4, D c = 3.881 g/cm 3 . The structure has been refined by full‐matrix least squares method to a final R factor of 0.064 for 2652 reflections collected at room temperature. The heteropoly anion contains two α‐B‐SbW 9 O 32 subunits joined by three square‐pyramidal CuO 4 (OH 2 ).