Syntheses, Crystal Structures and Characterization of Two Zeotype Crystals of 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

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....

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Veröffentlicht in:Chemical research in Chinese universities 2007, Vol.23 (1), p.8-13
1. Verfasser: ZHANG Xin YOU Wan-sheng ZHU Zai-ming DANG Li-qin SUN Zhen-gang ZHENG Xue-fang
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Sprache:eng
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Zusammenfassung: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.
ISSN:1005-9040
2210-3171