摘要
The heteropolytungstate(NH_4)_(20)[Na_2(H_2O)_2Ni(H_2O)_5{Ni(H_2O)}_2As_4W_(40)O_(140)] · 61H_2O is obtained by thereaction of Na_(27)[NaAs_4W_(40)O_(140)] · 60H_2O with NiCl_2 · 6H_2O and NH_4Cl in pH ≈ 4.0. Thestructure and chemical composition are determined by X-ray diffraction analysis and elementanalysis. The crystal data and main structure refinement are: a = 1.33135(18) nm, b = 1.9722(3) nm,c = 3.6430(5) nm, a = 78.010(2)°, β = 82.145(2)°, γ= 74.385(2)°, V= 8.978(2) nm^3, tricliniccrystal system, space group: P_1, Z= 2, R1 = 0.0512, and wR2 = 0.0684(I > 2σ). The four S2 sites ofthe big cyclic ligand [As_4W_(40)O_(140)]^(28-) are occupied by two Na^+ and two Ni^(2+)respectively, and each site supplies four O_d coordinating to metal ion. The coordination number ofNi^(2+) is six, and that of two Na^+ is five and six respectively. The third Ni^(2+) locates outsidethe cyclic [As_4W_(40)O_(140)]^(28-) and connects with one O_d, and its coordination number is six.
The heteropolytungstate (NH4)20[Na2(H2O)2Ni(H2O)5{Ni(H2O)}2As4W40O140]·61H2O is obtained by the reaction of Na27[NaAs4W40O140]·60H2O with NiCl2·6H2O and NH4Cl in pH≈4.0. The structure and chemical composition are determined by X-ray diffraction analysis and element analysis. The crystal data and main structure refinement are: a = 1.33135(18) nm, b = 1.9722(3) nm, c = 3.6430(5) nm, a = 78.010(2)? b = 82.145(2)? g = 74.385(2)? V = 8.978(2) nm3, triclinic crystal system, space group: P1, Z = 2, R1 = 0.0512, and wR2 = 0.0684(I >2). The four S2 sites of the big cyclic ligand [As4W40O140]28- are occupied by two Na+ and two Ni2+ respectively, and each site supplies four Od coordinating to metal ion. The coordination number of Ni2+ is six, and that of two Na+ is five and six respectively. The third Ni2+ locates outside the cyclic [As4W40O140]28- and connects with one Od, and its coordination number is six.
基金
This work was supported by the Foundation of Shaanxi Key Laboratory of Chemical Reaction Engineering.
