杂多酸盐K_4H[SiMO_(11)VO_(40)]·18H_2O 1和K_4H_2[PMo_9V_3O_(40)]·18H_2O 2的晶体结构

CRYSTAL STRUCTURE OF K_4H[SiMo_(11)VO_(40)]·18H_2O(1)AND K_4H_2[PMo_9V_3O_(40)]·18H_2O(2)

在-90℃下用X线单晶衍射法测定了标题化合物的晶体结构。晶体属P_(421)~c〔P4/mnc〕,α=12.540(2)〔12.515(3)〕,c=17.565(5)〔17.636(7)〕A,z=2.用1672〔788〕个独立可观测反射精修结构参数得R=0.059〔0.057〕。1中的Si是4配位。Si-O=1.58A。M(M=Mo,V)是6配位,M-O=1.64-2.37A。K是7配位,K-O=2.80～3.11A。在化合物2中,PO_4是无序的,P-O=1.51A,M-O=1.63～2.47A,K是7配位,K-O=2.85～3.10A。两个晶体都是多层二维的网状结构。

The crystal structures of the title compounds were determined by single crystal X-raydiffractometry at - 90℃。The complexes crystallize in tetragonal space groups P42_1c[P4/ mnc] with Z = 2[2]. Lattice parameters are a = 12.540(2) [12.515(3)], c = 17.565(5) [17.636(7)]A, V = 2762 (1) [2762 (2)]A~ε. The structures were solved by direct methods and Fouriertechniques and refined by least-squares techniques to R = 0.059[0.057] for 1672[788]reflec-tions. Si in compound (1) is 4-coordinated, Si-O = 1.58A. M(M = Mo, V) is 6-coordinated,M-O = 1.64 - 2.37A. K is 7-coordinated, K-O = 2.80--3.11A. In compound (2), PO_4 isdisordered, P-O = 1.51A, M-O = 1.63--2.47A, K is 7-coordinate, K--O = 2.85～3.10A. Bothstructures are in network.