On the polymorphism of aspirin

Angewandte Chemie - International Edition

Volumn 46, Issue 4, 2007, Pages 615-617

  Bond, Andrew D ^c   Boese, Roland ^a   Desiraju, Gautam R ^b  

^a UNIVERSITY OF DUISBURG ESSEN   (Germany)

^b UNIVERSITY OF HYDERABAD   (India)

^c UNIVERSITY OF SOUTHERN DENMARK   (Denmark)

Author keywords

Aspirin; Polymorphism; Structure determination; X ray diffraction

Indexed keywords

CRYSTAL STRUCTURE; DATA REDUCTION; REDUCTION; X RAY DIFFRACTION;

POLYMORPHISM; RE INDEXING; STRUCTURE DETERMINATION;

DRUG PRODUCTS;

ACETYLSALICYLIC ACID;

ARTICLE; CHEMICAL STRUCTURE; CHEMISTRY; CRYSTALLIZATION; X RAY CRYSTALLOGRAPHY;

ASPIRIN; CRYSTALLIZATION; CRYSTALLOGRAPHY, X-RAY; MOLECULAR STRUCTURE;

EID: 33846509337     PISSN: 14337851     EISSN: None     Source Type: Journal    
DOI: 10.1002/anie.200602378     Document Type: Article

References (18)

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12. int = 0.0255), 1756 observed reflections, R1-[I > 2σ(I)] = 0.0330, wR2(all data) = 0.0925, S = 1.08. CCDC 610952 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.a-c.uk/data_request/cif.
13. Full details of our experimental procedures are available in the Supporting Information. To put aside any question of experimental issues, crystal quality, etc. we note that the PZ result can be obtained purely by manipulation of data simulated from the form I structure. If the simulated single-crystal data set is subjected to the transformation [1 0 1/2 0 -1 0 0 0 -1], the form II structure can be refined against the transformed data to emulate the PZ result.
14. G. M. Sheldrick, SHELXS-97. University of Göttingen, Germany, 1997.
15. iso values. Of course, the R-factors are high. Acceptable R-factors can be obtained by application of a 2σ(I) cut-off. The fact that PZ did not report this issue suggests that some of their odd l reflections were non-zero at the 2σ(I) level.
16. It is very difficult to assess just how unusual this is. We note only that in our combined experience of many crystal-structure analyses, this is the first such example that we have identified.
17. G. R. Desiraju, Chem. Commun. 2005, 2995.
18. iso values, and the (supposed) necessity for an unacceptable 2θ cutoff. All these indicators are flagged as suspicious within an automated checking system such as checkCIF/PLATON.