Direct Structure Determination of a Multicomponent Molecular Crystal Prepared by a Solid-State Grinding Procedure

Journal of the American Chemical Society

Volumn 125, Issue 48, 2003, Pages 14658-14659

  Cheung, Eugene Y ^a   Kitchin, Simon J ^a   Harris, Kenneth D M ^a   Imai, Yoshitane ^b,c   Tajima, Nobuo ^b,c   Kuroda, Reiko ^b,c  

^a UNIVERSITY OF BIRMINGHAM   (United Kingdom)

^b UNIVERSITY OF TOKYO   (Japan)

^c JAPAN SCIENCE AND TECHNOLOGY AGENCY   (Japan)

Author keywords

[No Author keywords available]

Indexed keywords

ARTICLE; CRYSTALLIZATION; DENSITY; DIFFRACTION; GENETIC ALGORITHM; HYDROGEN BOND; MOLECULAR INTERACTION; NONHUMAN; NUCLEAR MAGNETIC RESONANCE; SOLID; SOLID STATE; STOICHIOMETRY; STRUCTURE ANALYSIS; X RAY DIFFRACTION;

EID: 0344861922     PISSN: 00027863     EISSN: None     Source Type: Journal    
DOI: 10.1021/ja030506s     Document Type: Article

References (26)

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9. (b) Imai, Y.; Tajima, N.; Sato, T.; Kuroda, R. Chirality 2002, 14, 604.
10. Unusually, it was possible in this case to determine the structures of both cocrystals from single-crystal X-ray diffraction data, as a single crystal of the phase obtained by solid-state grinding was, on one occasion, found as a very minor component during crystallization from solution.
11. Harris, K. D. M.; Tremayne, M.; Kariuki, B. M. Angew. Chem., Int. Ed. 2001, 40, 1626.
12. Harris, K. D. M.; Tremayne, M.; Lightfoot, P.; Bruce, P. G. J. Am. Chem. Soc. 1994, 116, 3543.
13. Grinding was carried out manually using a mortar and pestle, typically for 60 min. Depending on the relative amounts of the pure phases, the material obtained following grinding can contain residual amounts of one or more of the pure phases. Extensive trials using different relative amounts of the pure phases established the conditions for obtaining a single phase of the rac-BN/BQ/AN cocrystal. A slight excess of the pure phase of BQ (in comparison with the stoichiometry of the cocrystal) was necessary to produce the cocrystal as a single phase, compensating for partial sublimation of BQ during grinding.
14. The colour of the product phase (reddish purple) is markedly different from those of the pure phases of the individual components: BQ (yellow), BN (white), AN (white).
15. In contrast, for the rac-BN/BQ/naphthalene system, the same material is formed from both solution crystallization and solid-state grinding.1g
16. 1 (Gemonochromated); linear position-sensitive detector covering 8° in 2θ; 2θ range, 3.5°-50°: step size, 0.019°; data collection time, 10 h].
17. Visser, J. W. J. Appl. Crystallogr. 1969, 2, 89, 95.
18. (a) Kariuki, B. M.; Serrano-González, H.; Johnston, R. L.; Harris, K. D. M. Chem. Phys. Lett. 1997, 280, 189.
19. (b) Harris, K. D. M.; Johnston, R. L.; Kariuki, B. M. Acta Crystallogr. 1998, A54, 632.
20. (c) Turner, G. W.; Tedesco, E.; Harris, K. D. M.; Johnston, R. L.; Kariuki, B. M. Chem. Phys. Lett. 2000, 321, 183.
21. (d) Habershon, S.; Harris, K. D. M.; Johnston, R. L. J. Comput. Chem. 2003, 24, 1766.
22. (e) Cheung, E. Y.; McCabe, E. E.; Harris, K. D. M.; Johnston, R. L.; Tedesco, E.; Raja, K. M. P.; Balaram, P. Angew. Chem., Int. Ed. 2002, 41, 494.
23. Harris, K. D. M.; Johnston, R. L.; Habershon, S.; Turner, G. W.; Hanson, A.; Cheung, E. Y.; Kariuki, B. M.; Tedesco, E. EAGER, University of Birmingham, UK, 2003.
24. Larson, A. C.; Von Dreele, R. B. GSAS, Los Alamos Laboratory Report No. LA-UR-86-748, 1987.
25. wp in each subpopulation were copied into the other subpopulation with 80% probability.
26. p = 0.0209; 112 refined variables, 2438 profile points.