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Powder X-ray diffraction of bendamustine hydrochloride monohydrate, C16H22Cl2N3O2Cl·H2O

Published online by Cambridge University Press:  27 December 2018

J. A. Kaduk Open the ORCID record for J. A. Kaduk [Opens in a new window] ,
K. Zhong ,
T. N. Blanton ,
S. Gates-Rector  and
T. G. Fawcett
J. A. Kaduk
Affiliation:
Illinois Institute of Technology, 3101 S. Dearborn St., Chicago, IL 60616, USA
K. Zhong
Affiliation:
International Centre for Diffraction Data, 12 Campus Blvd., Newtown Square, PA, 19073-3273, USA
T. N. Blanton*
Affiliation:
International Centre for Diffraction Data, 12 Campus Blvd., Newtown Square, PA, 19073-3273, USA
S. Gates-Rector
Affiliation:
International Centre for Diffraction Data, 12 Campus Blvd., Newtown Square, PA, 19073-3273, USA
T. G. Fawcett
Affiliation:
International Centre for Diffraction Data, 12 Campus Blvd., Newtown Square, PA, 19073-3273, USA
*
a)Author to whom correspondence should be addressed. Electronic mail: tblanton@icdd.com
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Extract

Bendamustine hydrochloride monohydrate (marketed as Treanda®) is a nitrogen mustard purine analog alkylator used in the treatment of chronic lymphocytic leukemia (CLL) and non-Hodgkin lymphomas. Commercial bendamustine hydrochloride monohydrate crystallizes in the monoclinic space group P21/c (14), with a = 4.71348(4) Å, b = 47.5325(3) Å, c = 8.97458 (5) Å, β = 96.6515(8)°, V = 1997.161(23) Å3, and Z = 4. A reduced cell search in the Cambridge Structural Database yielded a previously reported crystal structure (Allen, 2002), which did not include hydrogens (Reck, 2006). In this work, the sample was ordered from Santa Cruz Biotechnology, and analyzed as received. The room-temperature crystal structure was refined using synchrotron (λ = 0.413896 Å) powder diffraction data, density functional theory (DFT), and Rietveld refinement techniques. Hydrogen positions were included as part of the structure, and recalculated during the refinement. The diffraction data were collected on beamline BM-11 at the Advanced Photon Source, Argonne National Laboratory. Figure 1 shows the powder X-ray diffraction pattern of the compound. The pattern is included in the Powder Diffraction File as entry 00-064-1508.

Keywords

bendamustine hydrochloride monohydrateX-ray diffractionpowder diffraction file
Type
Rapid Communication
Information
Powder Diffraction , Volume 34 , Issue 1 , March 2019 , pp. 74 - 75
Copyright
Copyright © International Centre for Diffraction Data 2018 

Bendamustine hydrochloride monohydrate (marketed as Treanda®) is a nitrogen mustard purine analog alkylator used in the treatment of chronic lymphocytic leukemia (CLL) and non-Hodgkin lymphomas. Commercial bendamustine hydrochloride monohydrate crystallizes in the monoclinic space group P21/c (14), with a = 4.71348(4) Å, b = 47.5325(3) Å, c = 8.97458 (5) Å, β = 96.6515(8)°, V = 1997.161(23) Å3, and Z = 4. A reduced cell search in the Cambridge Structural Database yielded a previously reported crystal structure (Allen, Reference Allen2002), which did not include hydrogens (Reck, Reference Reck2006). In this work, the sample was ordered from Santa Cruz Biotechnology, and analyzed as received. The room-temperature crystal structure was refined using synchrotron (λ = 0.413896 Å) powder diffraction data, density functional theory (DFT), and Rietveld refinement techniques. Hydrogen positions were included as part of the structure, and recalculated during the refinement. The diffraction data were collected on beamline BM-11 at the Advanced Photon Source, Argonne National Laboratory. Figure 1 shows the powder X-ray diffraction pattern of the compound. The pattern is included in the Powder Diffraction File as entry 00-064-1508.

Figure 1. (Color Online) Powder X-ray diffraction pattern of bendamustine hydrochloride monohydrate.

Use of the Advanced Photon Source at Argonne National Laboratory was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

This work was partially supported by the International Centre for Diffraction Data.

We thank Lynn Ribaud for his assistance in data collection.

SUPPLEMENTARY MATERIAL

The supplementary material for this article can be found at https://doi.org/10.1017/S0885715618000830.

References

Allen, F. H. (2002). The Cambridge Structural Database: a quarter of a million crystal structures and rising, Acta Cryst. Sect. B: Struct. Sci. 58, 380–388. CSD Refcode NEQGUM.Google Scholar
Reck, G. (2006) (Federal Institute of Materials and Research Testing, Berlin). Private communication.Google Scholar
Figure 0

Figure 1. (Color Online) Powder X-ray diffraction pattern of bendamustine hydrochloride monohydrate.

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