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利用常规合成方法制备了一个四核镍夹心型锑钨酸盐H_(10)[Ni_4~Ⅱ(H_2O)_(10)(B—β—SbW_9O_(33))_2]·2H_2O。晶体衍射数据显示,该化合物属于单斜晶系,P 21/n空间群,a=12.5088 (12)(?),b=12.7578(12)(?),c=29.318(3)(?),β=101.3340(10)°,V=4587.5(8)(?)~3,Z=2,R_1 =1.092,wR_2=0.2941。晶体解析表明,该多阴离子[Ni_4~Ⅱ(H_2O)_(10)(B—β—SbW_9O_(33))_2]~(10-)(简称Ni_4(H_2O)_(10)Sb_2W_(18))由2个[SbW_9O_(33)]~(9-)亚单元和四核Ni~Ⅱ离子[Ni_4~Ⅱ(H_2O)_(10)]~(8+)连接形成的。相邻的Ni_4(H_2O)_(10)Sb_2W_(18)之间通过弱的氢键作用连接形成二维层状结构。
A tetranuclear nickel sandwiched antimony tungstate H_ (10) [Ni_4 ~ Ⅱ (H_2O) _ (10) (B-β-SbW_9O_ (33)) _2] · 2H_2O was prepared by the conventional synthesis method. The crystal diffraction data show that the compound belongs to the monoclinic space group P 21 / n with a = 12.5088 (12) (?), B = 12.7578 (12) and c = 29.318 (3) β = 101.3340 (10) °, V = 4587.5 (8) (?) ~ 3, Z = 2, R_1 = 1.092, wR_2 = 0.2941. The crystal analysis shows that the polyanion [Ni_4 ~ Ⅱ (H_2O) _ (10) (B_β-SbW_9O_ (33)) _2] ~10 ~ (Ni_4 (H_2O) _ (10) Sb_2W_ (18) It is formed by the junction of two [SbW_9O_ (33)] ~ (9-) subunits and tetranuclear Ni ~ Ⅱ ions [Ni_4 ~ Ⅱ (H_2O) _ (10)] ~ (8+). The adjacent Ni_4 (H_2O) _ (10) Sb_2W_ (18) are connected by weak hydrogen bonds to form two-dimensional layered structure.