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Synthesis, Spectroscopic Properties and Structural Characterization of Sodium Potassium Citrato Oxotungstate(VI) Dimer
Affiliation:Department of Chemistry and State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen University, Xiamen, 361005;Department of Chemistry and State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen University, Xiamen, 361005;Department of Chemistry and State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen University, Xiamen, 361005;Department of Chemistry and State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen University, Xiamen, 361005;Department of Chemistry and State Key Laboratory for Physical Chemistry of Solid Surface, Xiamen University, Xiamen, 361005
Abstract:The sodium-potassium citrato oxotungstate(VI) dimer, Na4K2[W2O5-(VI) and excess potassium citrate monobasic (KH3cit) in neutral solution. The crystal data for the title compound.: monoclinic, C12H30K2Na4W2O30, Mr= 1192. 21, space groupP21/n, a=17.427(4), b=10.022(2), c=18.637(3) A, β=92.62(1)°, V=3252 (2) A3, Z=4, Dc=2. 435 g/cm3, μ(MoKa)=76.38 cm-1, F(000)=2288.The structure was refined to R= 0. 0434 for 6327 independent observed reflections with I > 3σ (I). The complex anion contains a quasi-centrosymmetric (O2W)Ob (WO2) core with a bent bridging oxo group [W-Ob-W 175.0(4)°]. Each citrate as tridentate ligand coordinates to a tungsten atom through the alkoxy, α-carboxyl, and oneβ-carboxyl group, while the other β-carboxyl group remains uncoordinated. Principal dimensions are: W-Ob 1. 883(6) A, (W=O,)av 1.715(6) A, W-O (alkoxy) 1. 959(6) A , W-O (α-carboxy) 2. 176(6) A and W-O (β-carboxy) 2.231(6) A. The tungsten atom is located in a distorted-octahedron environment.
Keywords:oxotungstate(VI)   citrate   citric acid   citrate method   crystal structure
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