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首页> 外文期刊>Journal of chemical crystallography >Structural determination by x-ray diffraction and W-183 NMR spectroscopy of mono substituted hexatungstates [(n-C4H9)(4)N](3)MW5O19 (M = Nb, V)
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Structural determination by x-ray diffraction and W-183 NMR spectroscopy of mono substituted hexatungstates [(n-C4H9)(4)N](3)MW5O19 (M = Nb, V)

机译：通过单取代六钨酸盐[[n-C4H9）（4）N]（3）MW5O19（M = Nb，V）的X射线衍射和W-183 NMR光谱确定结构

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The tetrabutylammonium salt of mononiobotungstate [(n-C4H9)(4)N](3)NbW5O19 (1) and the tetrabutylammonium salt of monovanadotungstate [(n-C4H9)(4)N](3)VW5O19 (2) are isotypes; both crystallize in the monoclinic system, space group C2/c (N degrees 15) with Z = 8. The cell parameters for 1 are a = 30.4038(8) angstrom, b = 18.5948(8) angstrom, c = 27.3330(3) angstrom, beta = 112.4555(6)degrees, V = 14281.1(7) angstrom(3) and the final reliability factors are R = 0.043 and R-w = 0.047 for 5801 reflections. The cell parameters for 2 are a = 30.096(8) angstrom, b = 18.373(3) angstrom, c = 27.201(6) angstrom, beta = 112.402(14)degrees, V = 13906(5) angstrom(3) and the final reliability factors are R = 0.048 and R-w = 0.054 for 6122 reflections. Both anions, [NbW5O19]3- and [VW5O19]3- exhibit the Lindqvist structure of the parent hexatungstate anion. The six metal positions are disordered and for each metal site the occupation factor is close to 1/6 M (M = Nb, V) and 5/6 W. Furthermore the two compounds were characterized by IR in the solid state, and W-183 solution NMR. The W-183 spectrum of [NbW5O19]3- presents two resonances with relative intensities 4:1 in agreement with the C-4v symmetry of the anion.
机译：单硼钨酸盐[（n-C4H9）（4）N]（3）NbW5O19（1）的四丁基铵盐和单钒钨酸盐[[n-C4H9）（4）N]（3）VW5O19（2）的四丁基铵盐是同种型;两者均在单斜晶系系统中结晶，空间群C2 / c（N度15），Z =8。1的像元参数为a = 30.4038（8）埃，b = 18.5948（8）埃，c = 27.3330（3）埃，beta = 112.4555（6）度，V = 14281.1（7）埃（3），对于5801次反射，最终的可靠性因子为R = 0.043和Rw = 0.047。 2的像元参数为a = 30.096（8）埃，b = 18.373（3）埃，c = 27.201（6）埃，beta = 112.402（14）度，V = 13906（5）埃，对于6122次反射，最终的可靠性系数为R = 0.048和Rw = 0.054。两种阴离子[NbW5O19] 3-和[VW5O19] 3-均表现出母体六钨酸盐阴离子的Lindqvist结构。六个金属位置无序，并且每个金属位点的占据因子接近1/6 M（M = Nb，V）和5/6W。此外，这两种化合物的特征在于固态的IR和W- 183溶液NMR。 [NbW5O19] 3-的W-183光谱显示两个共振，相对强度为4：1，与阴离子的C-4v对称性一致。

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