The crystal structure of D-ribose - At last!

Angewandte Chemie - International Edition

Volumn 49, Issue 26, 2010, Pages 4503-4505

  Šišak, Dubravka ^a   McCusker, Lynne B ^a   Zandomeneghi, Giorgia ^a   Meier, Beat H ^a   Bläser, Dieter ^b   Boese, Roland ^b   Bernd Schweizer, W ^a,b   Gilmour, Ryan ^a,b   Dunitz, Jack D ^a,b  

^a ETH ZURICH   (Switzerland)

^b UNIVERSITY OF DUISBURG ESSEN   (Germany)

Author keywords

Disorder in crystals; NMR spectroscopy; Ribose; Solid state structures; X ray diffraction

Indexed keywords

CRYSTAL FORMS; CRYSTALLINE COMPOUNDS; D-RIBOSE; FURANOSE; NMR SPECTROSCOPY; PYRANOSE; SOLID-STATE STRUCTURES;

CRYSTALS; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; X RAY DIFFRACTION; X RAYS;

CRYSTAL STRUCTURE;

EID: 77953653734     PISSN: 14337851     EISSN: 15213773     Source Type: Journal    
DOI: 10.1002/anie.201001266     Document Type: Article

References (15)

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8. In direct-space methods, a trial structure is generated within the asymmetric unit using known chemical information (e.g. atomic connectivity, bond distances and angles), and a powder pattern is calculated and compared with the measured one to get an estimate of the structure's correctness. The model is then modified and the corresponding pattern calculated. If the fit of this new pattern is better, the "move" is accepted and the cycle is repeated (see Ref. [6] for more information on global optimization procedures). Of importance here is the fact that a starting structural model is required. We did not know which of the five possible structures (Scheme 1) ribose would adopt in the solid state, so different combinations of chains and rings were used as input to FOX. With two molecules in the asymmetric unit, the problem is a nontrivial one for powder methods. After many FOX runs, a ring structure seemed more likely, but it was not clear whether this was a five- or six-membered ring, and none of the structural models was significantly better than the others. A long and tedious process of generating difference electron density maps from various starting models eventually led to an approximate structure with one α- and one β-pyranose molecule in the asymmetric unit. Later, an alternative approach involving the combination of an approximate (but incorrect) model from FOX with the powder charge flipping algorithm (C Baerlocher, L. B. McCusker, L. Palatinus, Z. Kristallogr. 2007, 222, 47-53) led to the structure in a more straightforward manner.
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14. Although both known polymorphs of crystalline D-ribose contain α- and β-pyranose molecules, they should not be described as co-crystals. Since α- and -pyranose are in dynamic equilibrium (along with αm- and β-furanose) in the melt and in the solutions from which D-ribose has been crystallized, only a single component is present in the crystalline materials.
15. CCDC 768155 (Form I, powder diffraction), CCDC 768156 (Form. I single crystal from zone melting), and CCDC 768157 (Form II) contain 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.ac.uk/data- request/cif.)