Ab initio structure determination of LiCF3SO3 from X-ray powder diffraction data using entropy maximization and likelihood ranking

Abstract Entropy maximization combined with likelihood ranking has been applied to the determination of a previously unknown inorganic crystal structure—lithium triflate, LiCF 3 SO 3 —from X-ray powder diffraction data. This technique partitions the intensities of overlapping reflections in a rational fashion and has the potential to solve more complex structures from powder diffraction data than has been possible previously. Structure solution of LiCF 3 SO 3 by this technique revealed a partially determined structure which was completed via difference Fourier and Rietveld refinement methods. Final refinement of the structure involved the use of both X-ray and neutron powder diffraction data. The structure is in the monoclinic system, space group P2 1 c , a = 10.2432(2) A, b = 5.0591(1)A, c = 9.5592(3)A, β = 90.319(2)°.

[1]  P. Bruce,et al.  Materials chemistry communications. Ab initio determination of molecular structures using high-resolution powder diffraction data from a laboratory X-ray source , 1992 .

[2]  G. Bricogne.  A multisolution method of phase determination by combined maximization of entropy and likelihood. III. Extension to powder diffraction data , 1991 .

[3]  E. Castellano,et al.  Crystal structures of neodymium and holmium trifluoromethanesulfonate enneahydrated , 1985 .

[4]  G. Bricogne.  Maximum entropy and the foundations of direct methods , 1984 .

[5]  C. J. Gilmore,et al.  Developments in the MITHRIL direct methods program , 1988 .

[6]  W. David,et al.  Extending the power of powder diffraction for structure determination , 1990, Nature.

[7]  A. White,et al.  Structure and stereochemistry in 'f-block' complexes of high coordination number. VIII. The [M(unidentate)9] system. Crystal structures of [M(OH2)9] [CF3SO3]3, M = La, Gd, Lu, Y , 1983 .

[8]  P. Bruce,et al.  Determination of a molecular crystal structure by X-ray powder diffraction on a conventional laboratory instrument , 1992 .

[9]  C. Wilson,et al.  Crystal structure determination from low-resolution X-ray powder diffraction data , 1990 .

[10]  G. Bricogne,et al.  A multisolution method of phase determination by combined maximization of entropy and likelihood. I. Theory, algorithms and strategy , 1990 .

[11]  Anthony K. Cheetham,et al.  Structure determination and refinement with synchrotron X-Ray powder diffraction data , 1991 .

[12]  G. Sheldrick.  Phase annealing in SHELX-90: direct methods for larger structures , 1990 .

[13]  G. Bricogne,et al.  A multisolution method of phase determination by combined maximization of entropy and likelihood. IV. The ab initio solution of crystal structures from their X-ray powder data , 1991 .

[14]  Lars Eriksson,et al.  TREOR, a semi-exhaustive trial-and-error powder indexing program for all symmetries , 1985 .

[15]  W. Bragg,et al.  The Employment of contoured Graphs of Structure-Factor in Crystal Analysis , 1936 .

[16]  Armel Le Bail,et al.  Ab-initio structure determination of LiSbWO6 by X-ray powder diffraction , 1988 .