钨钼杂多酸及其盐与二甲基甲酰胺加合物的制备和性质研究

Syntheses and Properties of Adducts between Heteropoly Tungstic and Molybdic Acids and Their Salts and N,N-Dimethyl Formamide

合成了10种钨钼杂多酸及其盐与DMF的加合物,用IR光谱、Raman光谱、UV光谱、~1HNMR、TG-DTA和X射线衍射方法研究了加合物的性质。加合物中配体DMF以C=O键的氧作为配位原子,与杂多酸中的质子或杂多酸盐中的金属阳离子配合成键。IR光谱中ν_(c-o)的位移可作为配位键成键强度的判据。

The adducts between heteropoly tungstic and molybdic acids and their salts and N, N-dimethyl formamide (DMF) were synthesized and characterized by IR, Raman, UV-VS, 1H and 13C NMR spectrometry, TG-DTA thermal analysis and X-ray diffraction analysis. The IR and NMR spectra showed that the coordinating atom of DMF was oxygen of C = O bond, and the shift of C = O vibration frequency might be considered as the criterion of M-O bond strength. The organic ligands do not coordinate with heteropoly anions, but with protons in heteropoly acids by hydrogen-bond, or metal cations in heteropoly tungstates and molybdates by coordination bond. The X-ray diffraction analysis showed that the DMF adduct of CaPW is monoclinic, and its space group is C2k5-P21/n, with unit cell parameters; a = 12. 927(7) A, 6=33.850(9) A, c=17. 903(13) A, B=106.78(4), V=7500. 37 A3.The figure of merit is F=M9(0. 016, 38).