From order to disorder and return: Remarkable molecular and crystal dynamics in solid [(C5H5)2Co][PF6]

Organometallics

Volumn 15, Issue 22, 1996, Pages 4675-4677

  Braga, Dario ^a   Scaccianoce, Laura ^a   Grepioni, Fabrizia ^a   Draper, Sylvia M ^b  

^a UNIVERSITY OF BOLOGNA   (Italy)

^b TRINITY COLLEGE DUBLIN   (Ireland)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0039898089     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om9602421     Document Type: Article

References (24)

1. Braga, D. Chem. Rev. 1992, 92, 633.
2. Inorganic Materials; Bruce, D. W., O'Hare, D., Eds.; John Wiley & Sons: Chichester, U.K., 1992.
3. (a) Lehn, J. M. Angew. Chem., Int. Ed. Engl. 1990, 29, 1304.
4. (b) Whitesides, G. M.; Simanek, E. E.; J. P. Mathias, J. P.; Seto, C. T.; Chin, D. N.; Mammen, M.; Gordon, D. M. Acc. Chem. Res. 1995, 28, 37.
5. (c) Sharma, C. V. K.; Desiraju, G. R. In Perspective in Supramolecular Chemistry. The Crystal as a Supramolecular Entity; Desiraju, G. D., Ed.; Wiley: New York, 1996.
6. (a) Braga, D.; Grepioni; F. J. Chem. Soc., Chem. Commun. 1996, 571.
7. (b) Braga, D.; Grepioni, F. Acc. Chem. Res. 1994, 27, 51.
8. (a) Daniel, M. F.; Leadbetter, A. J.; Meads, R. E.; Parker, W. G. J. Chem. Soc., Faraday Trans. 1978, 74, 456.
9. (b) Sato, K., Katada, M.; Sano, H.; Konno, M. Bull. Chem. Soc. Jpn. 1984, 57, 2361.
10. (c) Fitzsimmons, B. W.; Sayer, I. J. Chem. Soc., Dalton Trans. 1991, 2907.
11. Parsonage, N. G.; Staveley, L. A. K. Disorder in Crystals; Clarendon Press: Oxford, U.K., 1978.
12. (a) Martinez, R.; Tiripicchio, A. Acta Crystallogr. Sect. C 1990, C46, 202.
13. (b) Webb, R. J.; Lowery, M. D.; Shiomi, Y.; Sorai, M.; Wittebort, R. J.; Hendrickson D. N. Inorg. Chem. 1992, 31, 5211.
14. 6]. The yellow crystals are stable in the air and in the mother liquor.
15. 6P; M = 334.08; crystal size 0.15 × 0.20 × 0.08 mm, F(000) = 664; Mo Kα radiation, λ = 0.710 69 Å; monochromator graphite; θ-range 2.0-25.0°. The computer programs SHELX86 (Sheldrick, G. M. Acta Crystallogr., 1990, A46, 467) and SHELX93 (Sheldrick, G. M. Program for Crystal Structure Determination; University of Gottingen, Göttingen, Germany, 1993) were used for structure solution and refinement. All atoms except the hydrogen atoms were treated anisotropically. Hydrogen atoms were added in calculated position in form I and refined riding on their respective C atoms, while in form II they were found in difference Fourier maps and refined. In form III, 24 positions for the C atoms were generated by symmetry from the three found independent positions; therefore, the occupancy factors of the C atoms were set to the values giving the electron density corresponding to 10 C atoms. For all molecular representations, the graphic program SCHAKAL93 (Keller, E. Graphical Representation of Molecular Models, University of Freiburg, Germany, 1993) was used,
16. 6P; M = 334.08; crystal size 0.15 × 0.20 × 0.08 mm, F(000) = 664; Mo Kα radiation, λ = 0.710 69 Å; monochromator graphite; θ-range 2.0-25.0°. The computer programs SHELX86 (Sheldrick, G. M. Acta Crystallogr., 1990, A46, 467) and SHELX93 (Sheldrick, G. M. Program for Crystal Structure Determination; University of Gottingen, Göttingen, Germany, 1993) were used for structure solution and refinement. All atoms except the hydrogen atoms were treated anisotropically. Hydrogen atoms were added in calculated position in form I and refined riding on their respective C atoms, while in form II they were found in difference Fourier maps and refined. In form III, 24 positions for the C atoms were generated by symmetry from the three found independent positions; therefore, the occupancy factors of the C atoms were set to the values giving the electron density corresponding to 10 C atoms. For all molecular representations, the graphic program SCHAKAL93 (Keller, E. Graphical Representation of Molecular Models, University of Freiburg, Germany, 1993) was used,
17. 6P; M = 334.08; crystal size 0.15 × 0.20 × 0.08 mm, F(000) = 664; Mo Kα radiation, λ = 0.710 69 Å; monochromator graphite; θ-range 2.0-25.0°. The computer programs SHELX86 (Sheldrick, G. M. Acta Crystallogr., 1990, A46, 467) and SHELX93 (Sheldrick, G. M. Program for Crystal Structure Determination; University of Gottingen, Göttingen, Germany, 1993) were used for structure solution and refinement. All atoms except the hydrogen atoms were treated anisotropically. Hydrogen atoms were added in calculated position in form I and refined riding on their respective C atoms, while in form II they were found in difference Fourier maps and refined. In form III, 24 positions for the C atoms were generated by symmetry from the three found independent positions; therefore, the occupancy factors of the C atoms were set to the values giving the electron density corresponding to 10 C atoms. For all molecular representations, the graphic program SCHAKAL93 (Keller, E. Graphical Representation of Molecular Models, University of Freiburg, Germany, 1993) was used,
18. (b) The reversibility of the two phase transitions was confirmed by collecting other data sets at 293 and 313 K on the same crystal specimen discussed herein as well as at 223, 293, and 313 K on another two crystal specimens taken from the same preparation batch. A detailed comparison of these results will be given in a future report, (c) F⋯H separations were evaluated on C-H bonds normalized to 1.08 Å; seven bonds shorter than 2.60 Å are present in both form I (three <2.45 Å), and form II (five <2.45 Å). F⋯H bonds were not evaluated in the disordered form III.
19. Gavezzotti, A. J. Am. Chem. Soc. 1983, 95, 5220.
20. DSC thermograms were measured on a Perkin-Elmer DSC-7 in sealed Al pans; 5.150 mg of crystals was taken from the same crystal batch used for the diffraction experiments. The repeated cycles of cooling and heating (scanning rate 5.0 deg/min) had histereses of 12.7 and 4.5 K, for the form I ⇔ form II and the form I ⇔ form III transitions, respectively.
21. Gavezzotti, A.; Filippini, G. J. Am. Chem. Soc. 1995, 117, 12299.
22. Braga, D.; Biradha, K.; Grepioni, F.; Pedireddi, V. R.; Desiraju, G. R. J. Am. Chem. Soc. 1995, 117, 3156.
23. Braga, D.; Grepioni, F.; Byrne, J. J.; Wolf, A. J. Chem. Soc., Chem. Commun. 1995, 1023. Braga, D.; Costa, A. L.; Grepioni, F.; L. Scaccianoce, Tagliavini, E. Organometallics 1996, 15, 1084.
24. Braga, D.; Grepioni, F.; Byrne, J. J.; Wolf, A. J. Chem. Soc., Chem. Commun. 1995, 1023. Braga, D.; Costa, A. L.; Grepioni, F.; L. Scaccianoce, Tagliavini, E. Organometallics 1996, 15, 1084.