首页> 中文期刊> 《高等学校化学研究(英文版)》 >Syntheses, Crystal Structures and Characterization of Two Zeotype Crystals of K4Cr3O(H2O)3(OOCH)62P2W18O62 ·9.5H2O and K4Cr3O(H2O)3(OOCH)6H3P2W17Co(H2O)O61·20H2O

Syntheses, Crystal Structures and Characterization of Two Zeotype Crystals of K4Cr3O(H2O)3(OOCH)62P2W18O62 ·9.5H2O and K4Cr3O(H2O)3(OOCH)6H3P2W17Co(H2O)O61·20H2O

         

摘要

Two novel zeotype crystals, K4[Cr3O(H2O)3(OOCH)6]2[P2W 18 O 62 ]·9.5H2O(1) and K4[Cr3O(H2O)3·(OOCH)6][H3P2W 17 Co(H2O)O 61 ]·20H2O(2), were synthesized and their structures were determined using X-ray single crystal diffraction. Crystal data: C 12 H 43 O 103.5 K4Cr6P2W 18 (1), hexagonal P6(3)/m, a =1.5895(2) nm, b=1.5895(2) nm, c=2.1620(4) nm, α=90°, β=90°, γ=120°, V=4.7305(13) nm3, Z=2, R1=0.0726, wR2=0.1542; C6H 57 O 98 K4Cr3CoP2W 17 (2), hexagonal %P%6(3)/mmc, a = 1.61328(3) nm, b=1.61328(3) nm, c=2.06613(9) nm, α=90°, β=90°, γ=120°, V=4.6570(2) nm3, Z=2, R1=0.0377, wR2=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 1 and lacunary Wells-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.

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