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Spectroscopic Investigation of the Ion -; Crystal Structure of
(X = Cl, Br) and have been prepared by reactions of X2V(N3S2) with sodium fluoride in acetonitrile suspensions in the presence of 15-crown-5 and benzo-15-crown-5, respectively.The 15-N-labeled complex was also prepared and characterized by 15N, 19F, and 51V NMR spectra, as well as by IR spectroscopy.Whereas the crystal structure of , owing to disorder of the crown ether molecule, could be refined only to an R-value of 0.16 (space group C2/m, Z = 4, a = 1995.4(11); b = 1016.2(6); c = 1047.2(8) pm; beta = 100.83(4) deg at -65 deg C), the crystal structure of the corresponding was determined without complications.Space group P21/c, Z = 4, 5565 observed independent reflexion.R = 0.036.Lattic dimensions at 20 deg C; a = 1198.9(6); b = 970.3(5); c = 1918.2(10) pm; beta = 93.74(3) deg.The compound forms ion pairs, in which the sodium atom is seven-coordinated by the oxygen atoms of the crown ether molecule, the fluorine atom and one chlorine atom of the trigonal-bipyramidal – unit.The vanadium atom is part of a planar VN3S2 ring; fluorine and two nitrogen atoms of the cyclothiazeno ring occupy the equatorial positions. – Keywords: Fluoro-Chloro-Cyclothiazeno Complexes of Vanadium, 15N NMR Spectra; 51V NMR Spectra, IR Spectra, Crystal Structure
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Reference£º
Chiral Catalysts,
Chiral catalysts – SlideShare