用中温水热技术合成了2种Keggin型钼磷多金属氧酸盐[Cd (phen) 3]2[PMo^Ⅴ Mo11^Ⅵ O40 ]和 H3O[ Co(phen)3]2[ PMo2^Ⅴ Mo10^Ⅵ O40](Ⅱ).通过元素分析、红外光谱、X射线单晶衍射对其进行了表征.结果表明:2种化合物均属于三斜晶系,P-1,空间群;化合物Ⅰ的晶胞参数a = 1. 200 5 (2) nm, b = 1. 327 8 (3) nm, c = 1. 356 7 ( 3 ) nm, α = 103.56(3)^*,β= 91.37(3)^*, γ = 97.72(3)^*, V = 2. 079 8(7) nm^3, Z = 1, R1 = 0.044 2, wR2 = 0. 140 3. 化合物Ⅱ的晶胞参数 a = 1. 207 9 (2) nm, b = 1. 380 4 (3) nm, c=1.4421(3)nm, α = 104.81(3)^*,β= 109.63(3)^*, γ= 93.13(3)^*, V=2. 163 3(8)nm^3,Z= 1,R1 = 0. 071 7, wR2 = 0. 234 1.
Two new unprecedented Keggin-type polyoxometalate [Cd (phen) 3]2[PMo^Ⅴ Mo11^Ⅵ O40 ]and H3O[ Co(phen)3]2[ PMo2^Ⅴ Mo10^Ⅵ O40] were synthesized at mild hydrothermal condition, and the structure was characterized by elemental analysis, single crystal X-ray diffraction and IR. Compound ( Ⅰ ) crystallized in the monoclinic, space group P -1, a = 1. 200 5 (2) nm, b = 1. 327 8 (3) nm, c = 1. 356 7 ( 3 ) nm, α = 103.56(3)^*,β= 91.37(3)^*, γ = 97.72(3)^*, V = 2. 079 8(7) nm^3, Z = 1, R1 = 0.044 2, wR2 = 0. 140 3. Compound ( Ⅱ) crystallized in the monoclinic, space group P- 1, a = 1. 207 9 (2) nm, b = 1. 380 4 (3) nm, c=1.4421(3)nm, α = 104.81(3)^*,β= 109.63(3)^*, γ= 93.13(3)^*, V=2. 163 3(8)nm^3,Z= 1,R1 = 0. 071 7, wR2 = 0. 234 1.