化学学报 ›› 1982, Vol. 40 ›› Issue (3): 193-200.    下一篇

论文

鹤草酚的晶体结构和分子结构

唐有祺, 李根培, 金祥林, 郝润蓉   

  1. 北京大学物理化学研究所物质结构研究室
  • 投稿日期:1980-06-21 发布日期:2013-06-03
  • 通讯作者: 唐有祺

THE CRYSTAL AND MOLECULAR STRUCTURE OF AGRIMOPHOL

TANO YOU-QI, LI GEN-PEI, JIN XIAG-LIN, HAO RUN-RONG   

  1. Laboratory for Structure of Matter, Institute of Physical Chemistry, Peking University
  • Received:1980-06-21 Published:2013-06-03

鹤草酚晶体属三斜晶系,空间群为PI,晶胞参数为a=9.901(3),b=11.195(4),c=11.752(4)Å,α=80.74(3),α=75.66(3),γ=76.46(3)°,晶胞内分子数Z=2.用SyntexP3/R3型四圆衍射仪收集到2891个独立衍射强度.以直接法SHELXTL解出晶体结构.结构参数的修正采用了块对角矩阵最小二乘法,最后得偏离因子R=5.7%.晶胞中含有d-,l-两种对映体分子,它们彼此以I连系组成外消旋体.每分子中的两个六环分别同相邻的氧共面,其双面角为14.2°.两个六环通过碳(sp3)桥相连,并由于形成分子内氢键O-H…O(分别为2.705Å和2.745Å)而限制了自由转动.

The crystal of agrimophol, C26H34O8, is triclinic, space group PI, with a=9.091(3),b=11.195(4),c=11.752(4) Å, α=80.74(3),β=75.66(3),Å=76.46(3)°,Dm 1. 29,(by flotation in KI/H20), Dm1. 29 g·cm-3 for Z=2. The three-dimensional intensity data(2891 independent reflections) were obtained with a Syntex P3/R3 automated four-circle diffractometer. The structure was solved by direct method with SHELXTL and refined by block-diagonal-least-square technique to a conventional R value of 5.7% with ω=1/σ2 for all reflections. The unit cell contains two transmolecules, which are different optical isomers and racemized. The two sig-member rings are planar with neighboring O respectively, and linked by a carbon(sp3)bridge 116.5°) and two hydrogen bonds O-H…O(2.705Åand 2.745Å).The dihedral angle between two planes(six-member rings) is 14.2°.