View PDF Version
 
DOI: 10.1039/A807829G (Paper) Reference Section for: Chem. Commun., 1998, 2751-2752

Ab initio structure determination of norbornene from powder diffraction data using molecular packing analysis method

(Note: The full text of this document is currently only available in the PDF Version )

Jinrong Min, Jordi Benet-Buchholz and Roland Boese

Abstract

The previously unknown crystal structre of the low temperature ordered phase of norbornene was solved from a set of powder diffraction data with severe preferred orientation collected on a laboratory X-ray diffractometer by first predicting the starting model by means of molecular packing analysis method, which was then refined against the experimental data by means of Rietveld method.

References

  1. A. N. Fitch and H. Jobic, J. Chem. Soc., Chem. Commun., 1993, 1516 RSC.
  2. J. Benet-Buchholz, T. Haumann and R. Boese, Chem. Commun., 1998, 2003 RSC.
  3. R. Boese and M. Nussbaumer, in Organic crystal chemistry, ed. E. W. Jones, Oxford University Press, Oxford, UK, 1994, p. 20 Search PubMed; V. R. Thalladi, H.-C. Weiss, D. Bläser, R. Boese, A. Nangia and G. R. Desiraju, J. Am. Chem. Soc., 1998, 120, 8702 Search PubMed.
  4. K. D. M. Harris and M. Tremayne, Chem. Mater., 1996, 8, 2554 CrossRef CAS; K. Shankland, W. I. F. David and T. Csoka, Z. Kristallogr., 1997, 212, 550 CAS.
  5. P.-E. Werner, L. Eriksson and M. Westdahl, J. Appl. Crystallogr., 1985, 18, 367 CrossRef CAS.
  6. The DSC investigation was performed on DuPont 9900 controlled by program General V2.2A, heating rate 2 °C min–1.
  7. The general procedure for the conventional method is: extracting structure factor amplitudes; structure solution (direct methods or patterson method), Fourier recycling and refinement by single crystal method; and finish with Rietveld refinement.
  8. D. E. Williams, Program mpa/mpg, Molecular Packing Analysis/Molecular Packing Graphics. Department of Chemistry, University of Louisville, Louisville, KY 40292, USA.
  9. H. M. Rietveld, J. Appl. Crystallogr., 1969, 2, 65 CrossRef CAS.
  10. D. E. Williams, Acta Crystallogr., Sect. A, 1971, 27, 452 CrossRef CAS.
  11. J. Rodriguez-Carvajal, in Collected Abstracts of Powder Diffraction Meeting, Toulouse, France, July 1990, p. 127 Search PubMed.
  12. W. A. Dollase, J. Appl. Crystallogr., 1986, 19, 267 CrossRef CAS.
  13. Siemens Analytical X-ray Instruments, Inc., 1994, Ver. 5.03.
  14. Crystal data for norbornene at 105 K: C7H10, M= 94.16, monoclinic, space group P21/c, a= 7.6011(7), b= 8.5985(8), c= 8.7290(8)Å, β= 97.313(3)°, V= 565.87(9)Å3, Z= 4, Dc= 1.105 g cm–3. Overall isotropic thermal parameter B= 3.2(1)Å2. Final Rietveld refinement converted to Rp= 4.66%, Rwp= 6.48%, Rb= 10.0%, Rexp= 2.00%, χ2= 10.5 for 35 variables and 715 reflections distributed over 6025 profile points. Bond lengths (Å): C(1)–C(2) 1.524(1), C(3)–C(4) 1.522(1), C(2)–C(3) 1.334(1), C(4)–C(5) 1.563(1), C(1)–C(6) 1.562(1), C(5)–C(6) 1.557(1), C(1)–C(7) 1.547(1), C(4)–C(7) 1.545(1). See http://www.rsc.org/suppdata/cc/1999/2751/ for listing of bond lengths and angles and atomic coordinates.
Click here to see how this site uses Cookies. View our privacy policy here.