配合物[Sb(mpo)2Cl]的合成及晶体结构(Hmpo = 2-巯基氧化吡啶)

标题化合物 C10H8ClN2O2S2Sb 由C5H5NH]SbCl4]与 2-巯基氧化吡啶钠盐(Nampo)反应制得。其结构通过元素分析、IR 进行了表征,用 X-射线衍射法测定了该化合物的晶体结构。结果表明,晶体属于三斜晶系, 空间群为 P1, Mr = 409.50, 晶体参数:a = 9.4022(6), b =10.2910(7), c = 14.4631(9) ?, α= 104.321(1), β = 96.978(1), γ = 90.179(1)?, V = 1345.09(15)?3, Z = 4, Dc = 2.022 g/cm3, μ = 2.553 mm–1, F(000) = 792。晶体结构用直接法解出, 经全矩阵最小二乘法修正,最终结构偏离因子 R = 0.0368, wR = 0.0854。化合物分子中, 锑与一个氯原子和两个配体 mpo 配位,形成五配位变形的四角锥构型配合物。在晶胞堆积图中,锑原子又与另一分子中的氯原子以次级键形式作用,形成缺位配位多面体构型。

Synthesis and Crystal Structure of [Sb(mpo)2Cl] (Hmpo = 2-Mercaptopyridine N-Oxide)

The title compound C10H8ClN2O2S2Sb was synthesized by the reaction of C5H5NH]SbCl4] with Nampo (Hmpo = 2-thiopyridine noxide). X-ray single-crystal structure analysis showed that the crystal is of triclinic, space group P1 with Mr = 409.50, a = 9.4022(6), b =10.2910(7), c = 14.4631(9) ?, α = 104.3210(10), β = 96.9780(10), γ = 90.1790(10)o, Z = 4, Dc = 2.022 g/cm3, μ = 2.553 mm–1, F(000) = 792, R = 0.0368 and wR = 0.0854. In the molecule, each antimony atom is coordinated with two sulfur, two oxygen and one chlorine atoms.