Crystal structure determination of Jatrorrhizine chloride

Abstract

Optimum resolution data of powder X-ray diffraction (PXRD) for Jatrorrhizine (Jat) were collected by an X' Pert Pro MPD diffractometer with an X'celerator detector under the stepwise scanning condition as 8.255 ms and 0.00836° per step, 2 range of 5°-80° and total scanning period of 8-10 min. Indexing of the crystal system and a search of the space group from the powder X-ray diffraction data were conducted by the computational crystallography method. The pilot crystal models of Jat were globally optimized with Monte Carlo method and then refined with the Rietveld method. In parallel with PXRD test, single crystals of Jat were cultured in an aqueous solution by a slow-decreasing temperature method, then its crystal structure was determined by single crystal X-ray diffraction (SCXRD). Both crystal structures from PXRD and SCXRD are identical. The results show that the crystal structure of Jat belongs to a monoclinic system and the space group P2 1 /c. The parameters of cell dimensions from PXRD are a =7.69 Å, b = 12.55 Å, c = 20.89 Å,  = 106.53°, Z = 4, and V = 1933.4 Å 3 , meanwhile the parameters from SCXRD are a = 7.72 Å, b = 12.61 Å, c =20.99 Å,  =106.38°, Z =4, and V =1961.3 Å 3 .Jatrorrhizine, crystal, structure, X-ray diffractionSingle crystal X-ray diffraction (SCXRD) is undoubtedly the most recognized tool for elucidating crystal with its high quality pattern resolution, and accurate crystal structure parameters. However, the requirement for sample size significantly confines SCXRD usage because sometimes it is difficult to culture single crystals, especially those greater than 0.1 mm 3 . For example, the research fields of polymer science and pharmaceutical science, related to macromolecular/molecular crystals, only polycrystalline powders suitable for powder X-ray diffraction are available mostly.In the last two decades, the great progress has been achieved in determining crystal structures from polycrystalline powder diffraction [1][2][3] . All computational crystallography techniques are developed for acquisition of high resolution data of neutron/ synchrotron radiation diffraction, therefore their applicability for laboratory powder X-ray diffractometers is greatly confined by the term "high resolution" of diffraction data. It is crucial to investigate the methodology and applicability of computational crystallography techniques for crystal structure determination from conventional laboratory powder X-ray diffraction data. Based on the data of a laboratory powder X-ray diffractometer, our laboratory determined the pilot crystal structure of 7-amino-desacetoxy-cephalosporanic acid, which is a key intermediate for the derivation of Cephalosporin's compounds [4] .Both the molecular formula and crystal structure of Jatrorrhizine chloride (Jat) were determined from an SCXRD pattern with direct method [5] , with no chemical reference information available, by Wang et al. in 1989 [6] , and Ghosh et al. in 1993 [7] .The results of Jat crystal structure and methodology of structure determination from dat...

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