A combined solid-state NMR and X-ray powder diffraction study of a stable polymorph of paclitaxel

Crystal Growth and Design

Volumn 5, Issue 5, 2005, Pages 1737-1742

  Harper, James K ^a   Barich, Dewey H ^a   Heider, Elizabeth M ^a   Grant, David M ^a   Franke, Roland R ^b   Johnson, James H ^b   Zhang, Yuegang ^c   Lee, Peter L ^c   Von Dreele, Robert B ^c   Scott, Brian ^d   Williams, Darrick ^d   Ansell, Gerald B ^d  

^a UNIVERSITY OF UTAH   (United States)

^b Natural Pharmaceuticals Inc (NPI)   (United States)

^c ARGONNE NATIONAL LABORATORY   (United States)

^d LOS ALAMOS NATIONAL LABORATORY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 25444445608     PISSN: 15287483     EISSN: None     Source Type: Journal    
DOI: 10.1021/cg030074x     Document Type: Article

References (43)

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2. 3, Z = 4, Z′ = 1.
3. 3, Z = 4, Z′ = 1.
4. 3, Z = 2, Z′ = 1. Manuscript in final preparation.
5. 3, Z = 2, Z′ = 1. We appreciate the referee's suggestion that this rather large asymmetric unit cell represents the present state of the art for a combined ab initio quantum and XRPD study of cyclodextrin (CD) and mefenamic acid. One should take note of the rather large number of bond and angle constraints that are found for CD and the relative percent errors of the Rietveld fit of about 10%.
6. 1 and the unit cell parameters are β = 99.730°, a = 9.661 Å, b = 28.275 Å, c = 19.839 Å.
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10. Ranitidine hydrochloride, marketed by Glaxo plc under the name Zantac is known to be polymorphic. In a recent patent litigation [Glaxo Inc. (1993), Plaintiff v. Novopharm Ltd. Defendant, No. 91-759-CTV-% BO United States District for the Easter District of California, Raleigh Division 1993 U. S. Dist. LEWIS 13928], Glaxo's patent protection on this polymorph has been challenged.
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24. Isotropic chemical shifts are used in Figure 2 for the sake of simplicity and because they illustrate the symmetry features and asymmetric unit populations necessary to obtain unit cell dimensions and distances. Refinement of specific angular and distance constraints in the baccatin moiety requires an iterative sequence of fitting together the CST and XRPD data.
25. Harper, J. K.; Barich, D. H.; Heider E. M.; Grant, D. M. Manuscript in preparation. Preliminary results were presented by D. M. Grant at the International Society of Magnetic Resonance meeting in Rhodes, Greece, August 19-23, 2001.
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27. Harper, J. K.; Facelli, J, C.; Barich, D. H.; McGeorge, G.; Mulgrew A. E.; Grant, D. M. J. Am. Chem. Soc. 2002, 124, 10589-10595. In this reference, both the conformational structure and the chemical shift tensors are shown to be relatively invariant in a variety of baccatin molecular systems. This earlier shift tensor information from a study of various baccatin moieties provides a critical constraint on the paclitaxel fit of the XRPD data in this study.
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