物理化学学报 >> 1987, Vol. 3 >> Issue (01): 97-101.doi: 10.3866/PKU.WHXB19870118

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低价钒化合物结构化学研究 Ⅰ. [VCL2·(THF)4]+[ZnCl3·THF]-的合成与晶体结构

张泽莹; 苏雅丽   

  1. 北京大学物理化学研究所
  • 收稿日期:1986-01-27 修回日期:1986-06-20 发布日期:1987-02-15
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THE SYNTHESIS AND CRYSTAL STRUCTURE OF [VCl2·(THF)4]+[ZnCl3·THF]-

Zhang Zeying; Su Yali   

  1. Institute of Physical Chemistry; Peking University
  • Received:1986-01-27 Revised:1986-06-20 Published:1987-02-15
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Abstract: The title compound has been synthesized under nitrogen atmosphere using V_2O_5 for the initiator by Schlenk techniques. It′s single crystal, which is very air and water-sensitive, was obtained and determined from three-dimensinal x-ray diffraction data collected by the four-circle diffractometer. The crystals are orth- orhombic with space group D_2~4-P_(212121) and unit cell constants a=0.909 nm, b=1.4909 nm, c=2.1635 nm and z=4.
We derived first the positional parameters of V, Zn, Cland O atoms by direct method using SHELXTL program. The coordinates of other the non-hyleast-squares refinement for all atoms gave a final discrepency factor R=0.0945 and RW=0.0674.
The result of structure analysis shows that the compound is composed of the octahedral cation [VCl_2·(THF)_4]~+ and the tetrahedral anion [ZnCl_3·THF]~-.
The reaction mechanism was discussed. The title compound is reaction product of VCl_3 with ZnCl_2 in THF.