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X-ray powder diffraction data for calcium(II)–naproxen complex (C28H26CaO6·2H2O)

Published online by Cambridge University Press:  20 May 2015

Jing Wang ,
Di Wu ,
Shan Shan Li ,
Pei Xiao Tang ,
Li Li Wang  and
Hui Li
Jing Wang
Affiliation:
College of Chemical Engineering, Sichuan University, Chengdu 610065, People's Republic of China
Di Wu
Affiliation:
College of Chemical Engineering, Sichuan University, Chengdu 610065, People's Republic of China
Shan Shan Li
Affiliation:
College of Chemical Engineering, Sichuan University, Chengdu 610065, People's Republic of China
Pei Xiao Tang
Affiliation:
College of Chemical Engineering, Sichuan University, Chengdu 610065, People's Republic of China
Li Li Wang
Affiliation:
College of Chemical Engineering, Sichuan University, Chengdu 610065, People's Republic of China
Hui Li*
Affiliation:
College of Chemical Engineering, Sichuan University, Chengdu 610065, People's Republic of China
*
a) Author to whom correspondence should be addressed. Electronic mail: lihuilab@sina.com

Abstract

X-ray powder diffraction data, unit-cell parameters, and space group for calcium(II)–naproxen complex, C28H26CaO6·2H2O, are reported [a = 36.918(2) Å, b = 5.655(6) Å, c = 12.505(6) Å, β = 91.263(2)°, cell volume V = 2610.47 Å3, Z = 4, and space group C2]. All measured lines were indexed and are consistent with the C2 space group. No detectable impurities were observed.

Keywords

X-ray powder diffractionnaproxencomplex

Information

Type
New Diffraction Data
Information
Powder Diffraction , Volume 30 , Issue 2 , June 2015 , pp. 185 - 187
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Copyright
Copyright © International Centre for Diffraction Data 2015 

I. INTRODUCTION

Calcium(II)–naproxen complex (Figure 1) is a new potential anti-inflammatory drug synthesized recently, which is a white powder at room temperature. Metal complexes of the anti-inflammatory drug naproxen as auxiliary ligand have been widely studied since they were found to be more active and desirable drugs than their parent drugs themselves (Sharma et al., Reference Sharma, Singla and Dhawan2003; Abuhijleh and Khalaf, Reference Abuhijleh and Khalaf2010). The title compound is also expected to have some biological activities and medicinal value.

Figure 1.

Structural formula of calcium(II)–naproxen complex.

Presently, the crystal structure of calcium(II)–naproxen complex has not been reported.

II. EXPERIMENTAL

A. Sample preparation

Sodium naproxen, prepared by adding naproxen (2.3 g or 0.01 mol) to a 100 ml ethanolic solution of NaOH (0.4 g or 0.01 mol) and drying under vacuum at 40 °C, was dissolved in water (100 ml). To it, CaCl2 (0.56 g) was added with constant stirring. The precipitates of the calcium(II)–naproxen complex (final yield, 76%), thus, formed were filtered, washed with cold water, and dried under vacuum to a constant weight. The sample was characterized by UV–vis, FTIR (KBr, cm-1): ν(O–H): 3415, νasy(COO): 1604, νsy(COO): 1395, ν(Ca–O): 484; TG-DTA: mass change: -6.76%, melting point: 137°C; mass spectrometry [the UV–vis; FTIR and TG-DTA spectra are as supplementary material (Fig. 1S–3S)].

B. Diffraction data collection and reduction

The X-ray powder diffraction measurements were performed on an X'Pert PRO diffractometer (PANalytical Co., Ltd., the Netherlands) equipped with a PIXcel one-dimensional (1D) detection system and CuKα radiation (generator setting, 40 kV and 40 mA). The diffraction data were recorded at room temperature with a step size of 0.013 13°2θ within 5° to 50° in 2θ. Data evaluation was mostly conducted using the Reflex module in the software package Material Studio 4.2 (Accelrys Co., Ltd., San Diego, CA) in the State Key Laboratory of Polymer Materials Engineering (Sichuan University, Chengdu, Sichuan, China).

The powder diffraction pattern was pretreated by subtracting the background, stripping off Kα 2 peaks, and smoothing. Indexing was carried out using peak positions obtained from the powder diffraction profiles by the X-Cell method, and then the indexing result was refined using Pawley refinement (Harris, Reference Harris2012; Pan et al., Reference Pan, Guo, Duan, Cheng and Li2012). MC/SA search algorithm in Powder Solve package (Engel et al., Reference Engel, Wilke, König, Harris and Leusen1999; Wu et al., Reference Wu, Tang, Pan, Cheng and Li2013) was used to constantly adjust the conformation, position, and orientation of the molecular groups in the unit cell, which was selected by the indexing step, in order to reduce the difference between the calculated and the measured diffraction data.

III. RESULTS

The experimental powder diffraction pattern is depicted in Figure 2. Indexing results show that calcium(II)–naproxen complex is monoclinic with space group C2 and unit-cell parameters: a = 36.918(2) Å, b = 5.655(6) Å, c = 12.505(6) Å, β = 91.263(2)°, unit-cell volume V = 2610.47 Å3, space group C2, and Z = 4 (Table I). After Pawley refinement, the unit-cell parameters of calcium(II)–naproxen complex were solved. All lines of powder data were indexed and consistent with the C2 space group.

Figure 2.

X-ray powder diffraction pattern of calcium(II)–naproxen complex.

Table I.

Indexed X-ray powder diffraction data of calcium(II)–naproxen complex, C28H26CaO6·2H2O. Only the peaks with I obs of 1 or greater are reported [a = 36.918(2) Å, b = 5.655(6) Å, c = 12.505(6) Å, β = 91.263(2)°, unit-cell volume V = 2610.47 Å3, Z = 4, and space group C2]. All measured lines were indexed and are consistent with the C2 space group. The d-values were calculated using CuKα 1 radiation (λ = 1.540 56 Å).

SUPPLEMENTARY MATERIALS AND METHODS

The supplementary material for this article can be found at http://www.journals.cambridge.org/PDJ.

ACKNOWLEDGEMENT

We acknowledge financial support by the National Development and Reform Commission and Education of China (Grant No. 2014BW011).

References

Abuhijleh, A. L. and Khalaf, J. (2010). “Copper(II) complexes of the anti-inflammatory drug naproxen and 3-pyridylmethanol as auxiliary ligand. Characterization, superoxide dismutase and catecholase – mimetic activities,” Eur. J. Med. Chem. 45, 3811–3817.CrossRefGoogle ScholarPubMed
Engel, G. E., Wilke, S., König, O., Harris, K. D. M., and Leusen, F. J. J. (1999). “Powder solve-a complete package for crystal structure solution from powder diffraction patterns,” J. Appl. Crystallogr. 32, 1169–1179.CrossRefGoogle Scholar
Harris, K. D. M. (2012). “Powder diffraction crystallography of molecular solids,” Top. Curr. Chem. 315, 133–178.CrossRefGoogle ScholarPubMed
Pan, Q. Q., Guo, P., Duan, J., Cheng, Q., and Li, H. (2012). “Comparative crystal structure determination of griseofulvin: powder X-ray diffraction versus single-crystal X-ray diffraction,” Chin. Sci. Bull. 57(30), 3867–3871.CrossRefGoogle Scholar
Sharma, J., Singla, A. K., and Dhawan, S. (2003). “Zinc–naproxen complex: synthesis, physicochemical and biological evaluation,” Int. J. Pharm. 260, 217–227.CrossRefGoogle ScholarPubMed
Wu, X. Q., Tang, P. X., Pan, Q. Q., Cheng, Q., and Li, H. (2013). “Crystal structure determination of three polycyclic compounds and comparative Rietveld refinement between MS and GSAS programs,” Chin. Sci. Bull., 58, 2430–2434.CrossRefGoogle Scholar
Figure 0

Figure 1. Structural formula of calcium(II)–naproxen complex.

Figure 1

Figure 2. X-ray powder diffraction pattern of calcium(II)–naproxen complex.

Figure 2

Table I. Indexed X-ray powder diffraction data of calcium(II)–naproxen complex, C28H26CaO6·2H2O. Only the peaks with Iobs of 1 or greater are reported [a = 36.918(2) Å, b = 5.655(6) Å, c = 12.505(6) Å, β = 91.263(2)°, unit-cell volume V = 2610.47 Å3, Z = 4, and space group C2]. All measured lines were indexed and are consistent with the C2 space group. The d-values were calculated using CuKα1 radiation (λ = 1.540 56 Å).

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