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Ab initio structure determination and Rietveld refinement of the crystal structure of (Pb0.6Cu0.4)Sr2PrCu207−x

Published online by Cambridge University Press:  10 January 2013

Ping Yang ,
K. Sivakumar ,
Hoong-Kun Fun ,
Tsong-Jen Lee ,
Huan-Chiu Ku  and
Chiou-Chu Lai
Ping Yang
Affiliation:
School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia
K. Sivakumar
Affiliation:
School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia
Hoong-Kun Fun*
Affiliation:
School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia
Tsong-Jen Lee
Affiliation:
Department of Physics, National Tsing Hua University, Hsinchu, 30043, Taiwan
Huan-Chiu Ku
Affiliation:
Department of Physics, National Tsing Hua University, Hsinchu, 30043, Taiwan
Chiou-Chu Lai
Affiliation:
Institute of Electronics, National Chiao Tung University, Hsinchu, 30039, Taiwan
*
c)Corresponding author.
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Abstract

Ab initio structure determination of new compound (Pb0.6Cu0.4)Sr2PrCu2O7−x was obtained at 300 and 100 K from X-ray powder diffraction data and refined by Rietveld technique. (Pb0.6Cu0.4)Sr2PrCu2O7−x has an isotypical structure with TlBa2CaCu2O7 (1212) at both 300 and 100 K. At 300 K, crystal data: (Pb0.522Cu0.4)Sr2PrCu206.53, Mr=681.293, tetragonal system, space group P4/lmmm, a = 3.8631(5)Å, c= 11.9134(2)Å, V= 177.79Å3, Z= 1, Dx, = 6.3631 g/cm3, μ=1036.549 cm−1 (λ=1.54051 Å), F(000) = 299.6, the structure was refined with 31 parameters to Rwp = 4.02%, Rp=2.96% for 3379 step intensities and Rb = 4.80%, Rf=5.17 for 143 reflections, “goodness of fit” S = 2.20. At 100 K, crystal data: (Pb0.547Cu0.4)Sr2PrCu2O6.89, Mr=692.232, tetragonal system, space group P4/mmm, a = 3.8580(2) Å, c= 11.8898(5) Å, Z=1, Dx = 6.4953 g/cm3, μ= 1053.235 cm−1 (λ=1.54051 Å), F(000) = 304.6, the structure was refined with 32 parameters to Rwp = 5.53%, Rp=4.22% for 2574 step intensities and Rb = 6.11%, Rf=5.31% for 111 reflection, “goodness of fit” S= 1.79. Moreover, the composition of Pb was refined to 0.522 at 300 K and to 0.547 at 100 K as compared with the stoichiometric composition 0.6.

Keywords

ab initio structure determinationRietveld analysispowder diffractionhigh Tc materialcrystalline structure
Type
Research Article
Information
Powder Diffraction , Volume 10 , Issue 3 , September 1995 , pp. 154 - 158
Copyright
Copyright © Cambridge University Press 1995

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Footnotes

a)Permanent address: National Laboratory of Solid State Microstructure Physics, Nanjing University, Nanjing 210008, PR. China.
b)On leave from: Department of Physics, Anna University, Madras 600025, India.

References

Cernik, R. J., Cheetham, A. K., Prout, C. K., Watkin, D. J., Wilkinson, A. P., and Willis, B. T. M. (1991). “The strucuture of cimetidine (C 10H16N6S) solved from synchrotron-radiation X-ray powder diffraction data,” J. Appl. Cryst. 24, 222–226.CrossRefGoogle Scholar
Clearfield, A., McCusker, L. B., and Rudolf, P. (1984). “Crystal structures from powder data. 1. Crystal structure of ZrKH(PO4)2,” Inorg. Chem. 23, 4679–4682.CrossRefGoogle Scholar
Hill, R. J. (1992). “Rietveld refinement round robin. I. Analysis of standard X-ray and neutron data for PbSO4,” J. Appl. Cryst. 25, 589–610.CrossRefGoogle Scholar
Ku, H. C., and Lai, C. C. (1993). “Magnetic order and superconductivity in the TlBa2(Ca1−xPrx)Cu2Cu2O7−δ, system,” Chin. J. Low Temp. Phys. 15, 13–17.Google Scholar
Lai, C. C., Chiou, B. S., Chen, Y. Y., Ho, J. C., and Ku, H. C. (1992). “Anamalous Pr ordering in the new TlBa2PrCu2O7−δ compound,” Physica C 202, 104–108.CrossRefGoogle Scholar
Lai, C. C. (1993). “Magnetic rare earth ordering and superconductivity of (Tl, Pb)-1212 system,” Ph.D thesis, Natl. Chiao Tung Univ., Hsinchu, 30039, Taiwan, pp. 16 and 69.Google Scholar
Lightfoot, P., Tremayne, M., Harris, K. D. M., and Bruce, P. G. (1992). “Determination of a molecular crystal structure by X-ray powder diffraction on a conventional laboratory instrument,” J. Chem. Soc, Chem. Commun. 1012–1013.Google Scholar
Lightfoot, P., Mehta, M. A., and Bruce, P. G. (1993). “Crystal structure of the polymer electrolyte poly(ethylene oxide)3:LiCF3SO3,” Science 262, 883–885.CrossRefGoogle ScholarPubMed
Lightfoot, P., Thomson, J. B., Little, F. J., and Bruce, P. G. (1994). “Ab initio determination of crystal structures by X-ray powder diffraction: Structure of Li29Zr9Nb3O40,” J. Mater. Chem. 4, 167–169.CrossRefGoogle Scholar
Louer, M., Plevert, J., and Louer, D. (1988). “Structure of KCaPO4.H2O from X-ray powder diffraction data,” Acta Cryst. B 44, 463–467.CrossRefGoogle Scholar
Manako, T., Shimakawa, Y. D., Kubo, Y., Satoh, T., and Igarashi, H. (1988). “Non-superconducting TlBa2YCu2O7 with a new crystal structure resembling superconducting YBa2Cu3O7,” Physica C, 156, 315–318.CrossRefGoogle Scholar
Martin, C., Bourgault, D., Michel, C., Hervieu, M., and Raveau, B. (1989). “TlBa2NdCu2O7 and TlBa2YCu2O7 two non-superconductive oxides with the “1212” structure,” Mod. Phys. Lett. B 3, 93–99.CrossRefGoogle Scholar
Nakajima, S., Kikuchi, M., Syono, Y., Kubayashi, N., and Muto, Y. (1990). “Superconductivity of high-Tc TlBa2Ca1−xRExCu2O7, (RE=Nd, Gd or Y) system,” Physica C 168, 57–62.CrossRefGoogle Scholar
Nardelli, M. (1983). “PARST: A system of Fortran routines for calculating molecular structure parameters from results of crystal structure analyses,” Comput. Chem. 7, 95–98.CrossRefGoogle Scholar
Pawley, G. S. (1981). “Unit-cell refinement from powder diffraction scans,” J. Appl. Cryst. 14, 357–361.CrossRefGoogle Scholar
Poole, C. P. Jr., Datta, T., and Farach, H. A. (1988). Copper Oxide Super-conductors (Wiley, New York), 89 pp.Google Scholar
Sakthivel, A., and Young, R. A. (1991). USER'S GUIDE to Programs DBWS-9006 and DBWS-9006PC for Rietveld Analysis of X-ray and Neutron Powder Diffraction Patterns, 17 September 1991 (School of Physics, Georgia Institute of Technology, Atlanta, GA 30332, USA).Google Scholar
Sheldrick, G. M. (1990). “Phase annealing in SHELXL-90: Direct methods for larger structures,” Acta Cryst. A 46, 467–473.CrossRefGoogle Scholar
Sheldrick, G. M. (1993). “SHELXL-93: A program for crystal structure refinement,” University of Goettingen, Germany.Google Scholar
Werner, P -E., Eriksson, L., and Westdahl, M. (1985). “TREOR, a semiexhaustive trial-and-error powder indexing program for all symmetries,” J. Appl. Cryst. 18, 367–370.CrossRefGoogle Scholar
Wilson, C. C., and Wadsworth, J. W. (1990). “Crystal structure determination from low-resolution X-ray powder diffraction data,” Acta Cryst. A 46, 258–262.CrossRefGoogle Scholar