Three inorg.-org.-inorg. hybrids of dipalladium-substituted ﾎｳ-Keggin silicodecatungstates with org. linkers of different lengths, TBA8[{(ﾎｳ-H2SiW10O36Pd2)(O2C(CH2)nCO2)}2] (n = 1 (II), 3 (III), and 5 (IV), TBA = [Bu4N]+), were synthesized by exchange of the acetate ligands in TBA4[ﾎｳ-H2SiW10O36Pd2(OAc)2] (ITBA) with malonic, glutaric, and pimelic acids, resp. The x-ray crystallog. anal. of II, IIIA (IIIA: III with DCE, DCE = 1,2-dichloroethane), and IVA (IVA: IV with 10DCE) revealed that the anion parts of II, IIIA, and IVA were inorg.-org.-inorg. hybrids composed of two dipalladium-substituted ﾎｳ-Keggin silicodecatungstates connected by two dicarboxylate ligands. In the crystal structure of IVA, 10 DCE mols. per polyanion were present in the vicinity of polyanions. Compd. IVB (IVB: IV with 0.2DCE) was obtained by the evacuation of IVA. The DCE sorption-desorption isotherms of IVB showed that the amt. of DCE sorbed was satd. at 10.5 mol mol-1, of which the amt. was close to that (10 mol mol-1) of crystallog. assigned DCE mols. In the DCE sorption-desorption isotherms, a low-pressure hysteresis was obsd. probably because of H-bonding interaction between DCE mols. and polyanions. The powder XRD pattern of IVA changed with decrease in the relative DCE vapor pressure to form IVC (IVC: IV with 0.7DCE) at P/P0 = 0.0. The in situ powder XRD study showed reversible structure transformation between IVA and IVC driven by the sorption-desorption of DCE. [on SciFinder(R)]
各種検索
サポート
ヘルプ