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高等学校化学研究 ›› 1992, Vol. 8 ›› Issue (3): 239-246.

• Articles • 上一篇    下一篇

Syntheses and Structures of Sil abridged Hafnocene Dichlorides

ZHOU Xiu-zhong1, WANG Ying1, XU Shan-sheng1, WANG Hong-gen2, YAO Xin-kai2   

  1. 1. Department of Chemistry, Nankai University, Tianjin, 300071;
    2. Central Laboratory, Nankai University, Tianjin, 300071
  • 收稿日期:1991-09-04 出版日期:1992-08-24 发布日期:2011-09-09

Syntheses and Structures of Sil abridged Hafnocene Dichlorides

ZHOU Xiu-zhong1, WANG Ying1, XU Shan-sheng1, WANG Hong-gen2, YAO Xin-kai2   

  1. 1. Department of Chemistry, Nankai University, Tianjin, 300071;
    2. Central Laboratory, Nankai University, Tianjin, 300071
  • Received:1991-09-04 Online:1992-08-24 Published:2011-09-09

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摘要： The present paper covers three silabridged hafnocene dichlorides(1, 2 and 3) prepared by sequential reactions of α, ω-dichloropermethyl polysilane with cyclopentadienyl sodium, n-butyl lithium and hafnium tetrachloride. Their structures were characterized by elemental analyses, UV, 1H(13C) NMR and MS. Furthermore the crystal and molecular structures of 1 and 2 were determined by X-ray diffraction method. The crystal of 1 is monoclinic, space group C2/c with a=1. 3401(4), b=0. 9977(3), c=1. 0922(4) nm; β=94. 07(1)° V=3. 6342 nm3, Z=2, Dc= 2.155 g·cm-3. The final deviation factor R=0. 064. The crystal of 2 is monoclinic, space group P21/c with a=0.0847(1), b=1.5181(1), c=2.9824(2) nm; β= 94. 07(1)°, V=3.634 nm3; Dc= l. 805 g·cm-3. The final deviation factor R=0. 033. The relationship between the silabridged structure and spectral properties is also discussed.

关键词: Silabridged hafnocene dichloride, Synthesis, Molecular structure

Abstract: The present paper covers three silabridged hafnocene dichlorides(1, 2 and 3) prepared by sequential reactions of α, ω-dichloropermethyl polysilane with cyclopentadienyl sodium, n-butyl lithium and hafnium tetrachloride. Their structures were characterized by elemental analyses, UV, 1H(13C) NMR and MS. Furthermore the crystal and molecular structures of 1 and 2 were determined by X-ray diffraction method. The crystal of 1 is monoclinic, space group C2/c with a=1. 3401(4), b=0. 9977(3), c=1. 0922(4) nm; β=94. 07(1)° V=3. 6342 nm3, Z=2, Dc= 2.155 g·cm-3. The final deviation factor R=0. 064. The crystal of 2 is monoclinic, space group P21/c with a=0.0847(1), b=1.5181(1), c=2.9824(2) nm; β= 94. 07(1)°, V=3.634 nm3; Dc= l. 805 g·cm-3. The final deviation factor R=0. 033. The relationship between the silabridged structure and spectral properties is also discussed.

Key words: Silabridged hafnocene dichloride, Synthesis, Molecular structure