Abstract
The reaction of Na 2WO 4·2H 2O, W(CO) 6 and GaCl 3 in 120°C propionic anhydride produced insoluble black crystals containing [W 3O 4(O 3CEt) 3] 4 bridged by Ga 3+ ions (1). They decompose in hot aqueous 2 M HCl solution to produce discrete [W 3O 4] 4+ cluster species. Cluster 1 was characterized by X-ray crystallography with the following crystal data: triclinic, space group P-1, a = 12.3715(5), b = 13.0356(6), c = 14.0021(6) A ̊ , α = 90.36(1), β = 109.70(1), γ = 117.69(1)°, V = 1646.1(1) A ̊ 3, Z = 1 . The structure consists of the two incomplete cuboidal units [W 3O 4(O 2CEt) 8] 4+, bridged by two Ga 3+ ions to form the centrosymmetric cyclic octanuclear dianion [W 3GaO 4(O 2CEt) 8] 2 2− . Alkali metal ions Na + further link the dianions into an infinite chain. The IR spectrum of the cluster is assigned.
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