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在硅凝胶中培养了标题配合物的单晶,确定了它的组成,并进行了热谱、可见光谱、红外光谱及其他多项物理性质的测试和表征,其结果与单晶X射线衍射分析的结果一致。晶体学数据:分子式[K(18-冠-6)(H_2O)][K(18-冠-6)][Cr(H_2O)(NCS)_5]·H_2O,空间群C_(2h)~5—P2_1/n,a=8.592(5),b=22.976(10),c=24.372(4)A,13=96.57(4)~0,Z=4。结构用直接法解出,全矩阵最小二乘方修正,R=0.046。结果表明,铬(Ⅲ)由五个异硫氯酸根离子和一水分子配位形成一畸变八面体形的配合阴离子。一个钾离子由一个冠醚和另一水分子配位;另一钾离子由另一冠醚和一配位于铬(Ⅲ)的硫氯酸根的硫原子配位,即该N(3)-C(3)-S(3)桥连在Cr和K(2)之间;两钾离子均是7配位。第三个水分子通过氢键与阴离子的配位水分子和两个冠醚环上的醚氧原子相连。
The single crystal of the title complex was grown in silica gel and its composition was determined. The thermal spectrum, visible spectrum, infrared spectrum and many other physical properties were tested and characterized. The results were in agreement with the single crystal X-ray diffraction The results of the analysis are consistent. Crystallographic data: Molecular formula: K [18-crown-6] (H_2O)] [K (18-crown-6)] [Cr (H_2O) (NCS) _5] P2_1 / n, a = 8.592 (5), b = 22.976 (10), c = 24.372 (4) A, 13 = 96.57 (4) ~ 0, Z = 4. The structure is solved by the direct method, the whole matrix least squares correction, R = 0.046. The results show that chromium (Ⅲ) is coordinated by five isothionate ions and one water molecule to form a distorted octahedron anions. One potassium ion is coordinated by one crown ether and another water molecule; the other potassium ion is coordinated by another crown ether with the sulfur atom of a chromite located on chromium (III), ie, the N (3) -C (3) -S (3) bridges between Cr and K (2); both potassium ions are 7-coordinated. The third water molecule is connected to the anodic coordination water molecule and the ether oxygen atoms of the two crown ether rings by hydrogen bonding.