Synthesis and crystal structure of a novel double 1:11 series arsenotungstate: [Cu I(phen) 2] 5H 6[Sm(AsW 11O 39) 2]·6H 2O

Abstract

A novel double 1:11 series arsenotungstate, [Cu I(phen) 2] 5H 6[Sm(AsW 11O 39) 2]·6H 2O (phen=1,10-phenanthroline) was synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The title compound was monoclinic, space group P2 1/ c, a=3.75710(2) nm, b=1.39776(8) nm, c=3.33735(18) nm, β =96.967(10)°, V=17.3969(17) nm 3, Z=4. Single crystal X-ray structural analyses revealed that the dimeric polyanion, [SmAs 2W 22O 78] 1–, consisted of one central Sm 3+ ion and two tetradentate heteropoly ligands [AsW 11O 39] 7–. The Sm 3+ ion and two tetradentate defective [AsW 11O 39] 7– anions were joined together by the sharing of four oxygen atoms from each heteropoly ligand. The bond valence sum (BVS) calculations of the title compound suggested that all four Cu atoms were in the +1 oxidation sate.