摘要
Two novel zeotype crystals, K4[Cr30（H2O） 3（OOCH） 6] 2[ P2W18O62]· 9.5H2 O and K4[ Cr3O（ H2O）3（ OOCH）6 ]2[ H3 P2 W17Co（H2O） O61]· 20H2O（2） , were synthesized and their structures were determined using X-ray single crystal diffraction. Crystal data： C12H43O103.5K4Cr6P2W18（1）, hexagonal P6（3）/m, α= 1. 5895（2） nm, b=1.5895（2） nm, c =2.1620（4） nm, α=90°, β=90°, γ= 120°, V=4.7305（13） nm^3, Z=2, R1 =0,0726, ωR2 =0. 1542; C6H57O98K4Cr3CoP2W17 （2）, hexagonal P6（3）/mmc, α = 1.61328（3） nm, b = 1.61328（3） nm, c=2.06613（9） nm, α=90°, β=90°, γ=120°, V=4.6570（2） nm^3, Z=2, R1 =0.0377, ωR2 =0. 1070. These crystals were characterized using elemental analysis, IR, TG-DTA, and XRD. It was found that the polyoxometalate anions maintained Wells-Dawson structure for crystal I and laeunary Wens-Dawson structure for crystal 2. Thermal analysis showed that crystal 1 lost the water of crystallization at 132 ℃, whereas crystal 2 lost the water of crystallization at 100 ℃. Crystal 1 could reversibly desorb and adsorb water molecules and its crystal structure could be restored after re-adsorbing the water molecules. It was also found from the XRD patterns that the void size of crystal 2 is smaller compared with that of crystal 1, which is attributed to the higher anion charges.
Two novel zeotype crystals, K4[Cr30（H2O） 3（OOCH） 6] 2[ P2W18O62]· 9.5H2 O and K4[ Cr3O（ H2O）3（ OOCH）6 ]2[ H3 P2 W17Co（H2O） O61]· 20H2O（2） , were synthesized and their structures were determined using X-ray single crystal diffraction. Crystal data： C12H43O103.5K4Cr6P2W18（1）, hexagonal P6（3）/m, α= 1. 5895（2） nm, b=1.5895（2） nm, c =2.1620（4） nm, α=90°, β=90°, γ= 120°, V=4.7305（13） nm^3, Z=2, R1 =0,0726, ωR2 =0. 1542; C6H57O98K4Cr3CoP2W17 （2）, hexagonal P6（3）/mmc, α = 1.61328（3） nm, b = 1.61328（3） nm, c=2.06613（9） nm, α=90°, β=90°, γ=120°, V=4.6570（2） nm^3, Z=2, R1 =0.0377, ωR2 =0. 1070. These crystals were characterized using elemental analysis, IR, TG-DTA, and XRD. It was found that the polyoxometalate anions maintained Wells-Dawson structure for crystal I and laeunary Wens-Dawson structure for crystal 2. Thermal analysis showed that crystal 1 lost the water of crystallization at 132 ℃, whereas crystal 2 lost the water of crystallization at 100 ℃. Crystal 1 could reversibly desorb and adsorb water molecules and its crystal structure could be restored after re-adsorbing the water molecules. It was also found from the XRD patterns that the void size of crystal 2 is smaller compared with that of crystal 1, which is attributed to the higher anion charges.
基金
Supported by the Dalian Municipal Science and Technology Commission and Liaoning Provincial Science and Technology Com-mission(No. 20031059)
