(enH_2)_4Na_4H_3[(VO)_(12)O_6B_(18)O_(42)]·8H_2O的水热合成和晶体结构

在水热的条件下合成了多钒硼酸盐(enH2)4Na4H3(VO)12O6B18O42]8H2O, 化学式为C8H59B18N8Na4O68V12 (Mr=2253.45), 用单晶X射线衍射方法测定了它的结构, 该晶体属单斜晶系, P21/n空间群, 晶胞参数为a = 13.8989(4), b = 16.1954(5), c = 14.4520(4) ?β = 94.7490(5), V= 3241.95(16) ?, Z = 2, Dc = 2.308 g/cm3, ?= 1.819mm-1, F(000) = 2234, 4798个可观察衍射点(I > 2s(I)), 最终结构精修到偏离因子R = 0.0449, wR = 0.1163, S = 0.996。在该化合物的结构中, V12B18簇是由环状的B18O42通过18个B(μ3-O)V键被2个V6O18环夹在中间组成的, V12B18簇通过4个Na+与相邻的簇相连, 形成二维网状结构, 孔道尺寸为6.109×10.562 拧?

Hydrothermal Synthesis and Crystal Structure of (enH2)4Na4H3[(VO)12O6B18O42]·8H2O

The title compound with formula C8H59B18N8Na4O68V12 (Mr = 2253.45) has been synthesized under hydrothermal condition and its crystal structure was determined by X-ray diffraction. It belongs to monoclinic, space group P21/n with a = 13.8989(4), b = 16.1954(5) c = 14.4520(4) ? b = 94.7490(5)? V = 3241.95(16) ?, Z = 2, Dc = 2.308 g/cm3, ?= 1.819 mm-1, F(000) = 2234 and S = 0.996. The final R and wR are 0.0449 and 0.1163, respectively for 4798 observed reflections with I > 2s(I). In the structure of the compound, the V12B18 cluster is composed of a B18O42 ring sandwiched between two vanadium-oxygen rings V6O18 by eighteen B(m3-O)V bonds, and these clusters are connected with Na+. Thus, the complex extends into an infinite two-dimensional network structure with the size of the hole being 6.109×10.562?