How to determine structures when single crystals cannot be grown: opportunities for structure determination of molecular materials using powder diffraction data.

Many crystalline solids cannot be prepared as single crystals of sufficient size and/or quality for structure determination to be carried out using single crystal X-ray diffraction techniques. In such cases, when only polycrystalline powders of a material are available, it is necessary instead to tackle structure determination using powder X-ray diffraction. This article highlights recent developments in the opportunities for determining crystal structures directly from powder diffraction data, focusing on the case of molecular solids and giving particular attention to the most challenging stage of the structure determination process, namely the structure solution stage. In particular, the direct-space strategy for structure solution is highlighted, as this approach has opened up new opportunities for the structure determination of molecular solids. The article gives an overview of the current state-of-the-art in structure determination of molecular solids from powder diffraction data. Relevant fundamental aspects of the techniques in this field are described, and examples are given to highlight the application of these techniques to determine crystal structures of molecular materials.

[1]  W. David.  On the number of independent reflections in a powder diffraction pattern , 1999 .

[2]  K. Harris,et al.  The application of a genetic algorithm for solving crystal structures from powder diffraction data , 1997 .

[3]  K. Roberts,et al.  Computationally Assisted Structure Determination for Molecular Materials from X-ray Powder Diffraction Data , 1997 .

[4]  Anthony K. Cheetham,et al.  The structure of cimetidine (C10H16N6S) solved from synchrotron-radiation x-ray powder diffraction data , 1991 .

[5]  W. Motherwell,et al.  Structure solution and refinement of tetracaine hydrochloride from X-ray powder diffraction data , 2002 .

[6]  A. McGhie,et al.  X-ray Powder Diffraction Structure of Triclinic C60Br24(Br2)2 , 1995 .

[7]  Kenneth D. M. Harris,et al.  Structure Determination of a Complex Organic Solid from X‐Ray Powder Diffraction Data by a Generalized Monte Carlo Method: The Crystal Structure of Red Fluorescein , 1997 .

[8]  Jonathan P. Wright,et al.  Solving larger molecular crystal structures from powder diffraction data by exploiting anisotropic thermal expansion. , 2003, Angewandte Chemie.

[9]  G. A. Slack,et al.  Organometallic precursors to aluminum nitride: synthesis and crystal structures of amidodimethylaluminum trimer and the planar species amidodi-tert-butylaluminum trimer , 1989 .

[10]  K. Harris,et al.  Rationalizing the structural properties of bupivacaine base--a local anesthetic--directly from powder X-ray diffraction data. , 2004, Journal of pharmaceutical sciences.

[11]  W. Pritzkow,et al.  POSIT – a method for structure determination of small partially known molecules from powder diffraction data.Structure of 6-methyl-1,2,3,4-tetrahydropyrimidine-2,4-dione (6-methyluracil) , 1988 .

[12]  Roy L. Johnston,et al.  C−H⋅⋅⋅O Hydrogen Bond Mediated Chain Reversal in a Peptide Containing a γ‐Amino Acid Residue, Determined Directly from Powder X‐ray Diffraction Data , 2002 .

[13]  Roy L. Johnston,et al.  Development of a multipopulation parallel genetic algorithm for structure solution from powder diffraction data , 2003, J. Comput. Chem..

[14]  William I. F. David,et al.  Crystal structure determination from powder diffraction data by the application of a genetic algorithm , 1997 .

[15]  K. Harris,et al.  An efficient algorithm for calculating whole-profile functions in crystal structure solution from powder diffraction data , 2004 .

[16]  D. Louër,et al.  Indexing of powder diffraction patterns for low-symmetry lattices by the successive dichotomy method , 1991 .

[17]  Kenneth D. M. Harris,et al.  Structural Properties of Self-Organized Organo-Silicon Macromolecular Films Investigated by Scanning Tunneling Microscopy and X-ray Diffraction , 2000 .

[18]  Kenneth D. M. Harris,et al.  CRYSTAL STRUCTURE DETERMINATION FROM POWDER DIFFRACTION DATA BY MONTE CARLO METHODS , 1994 .

[19]  D. Seebach,et al.  Cyclo‐β‐peptides: Structure and tubular stacking of cyclic tetramers of 3‐aminobutanoic acid as determined from powder diffraction data , 1997 .

[20]  K. Harris,et al.  Topochemical Rationalization of the Solid-State Polymerization Reaction of Sodium Chloroacetate: Structure Determination from Powder Diffraction Data by the Monte Carlo Method , 1997 .

[21]  T. Pilati,et al.  P‐RISCON: a real‐space scavenger for crystal structure determination from powder diffraction data , 1994 .

[22]  Wei Xu,et al.  Structure determination of enalapril maleate form II from high-resolution X-ray powder diffraction data. , 2003, Journal of pharmaceutical sciences.

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

[24]  Brian H. Toby,et al.  Solid State Lithium Cyanocobaltates with a High Capacity for Reversible Dioxygen Binding: Synthesis, Reactivity, and Structures , 1995 .

[25]  W. Zachariasen,et al.  The crystal structure of beta plutonium metal , 1963 .

[26]  Peter G. Bruce,et al.  A General Monte Carlo Approach to Structure Solution from Powder Diffraction Data: Application to Poly(ethylene oxide)3:LiN(SO3CF3)2 , 1997 .

[27]  R. Céolin,et al.  Tetramorphism of fananserine : p, T diagram and stability hierarchy from crystal structure determinations and thermodynamic studies , 2001 .

[28]  K. Shankland,et al.  Structural characterization of three crystalline modifications of telmisartan by single crystal and high-resolution X-ray powder diffraction. , 2000, Journal of pharmaceutical sciences.

[29]  A. Meden,et al.  Crystal Structure Solution from Powder Diffraction Data – State of the Art and Perspectives , 1998 .

[30]  K. Shankland,et al.  Molecular, crystallographic and algorithmic factors in structure determination from powder diffraction data by simulated annealing , 2002 .

[31]  Douglas Philp,et al.  Evolving Opportunities in Structure Solution from Powder Diffraction Data-Crystal Structure Determination of a Molecular System with Twelve Variable Torsion Angles. , 1999, Angewandte Chemie.

[32]  R. Dinnebier,et al.  New insights into an old reaction. High-resolution x-ray powder diffraction of Wiberg's aminoalane intermediate. , 2003, Inorganic chemistry.

[33]  John B. O. Mitchell,et al.  The determination of the crystal structure of anhydrous theophylline by X-ray powder diffraction with a systematic search algorithm, lattice energy calculations, and C-13 and N-15 solid-state NMR: A question of polymorphism in a given unit cell , 2001 .

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

[35]  R. Cernik,et al.  Ab initio structure determination of sulfathiazole polymorph V from synchrotron X-ray powder diffraction data , 1999 .

[36]  Roy L. Johnston,et al.  The genetic algorithm : Foundations and applications in structure solution from powder diffraction data , 1998 .

[37]  Roy L. Johnston,et al.  Structure Determination of an Oligopeptide Directly from Powder Diffraction Data , 2000 .

[38]  R. Peschar,et al.  A Monte Carlo approach to crystal structure determination from powder diffraction data , 2003 .

[39]  Gerhard M. J. Schmidt,et al.  Photodimerization in the solid state , 1971 .

[40]  K. Harris,et al.  Direct structure determination of a multicomponent molecular crystal prepared by a solid-state grinding procedure. , 2003, Journal of the American Chemical Society.

[41]  K. Harris,et al.  Contemporary Advances in the Use of Powder X-Ray Diffraction for Structure Determination. , 2001, Angewandte Chemie.

[42]  Peter W. Stephens,et al.  The structure of malaria pigment β-haematin , 2000, Nature.

[43]  G. S. Pawley,et al.  Unit-cell refinement from powder diffraction scans , 1981 .

[44]  W. Łasocha,et al.  Crystal structure of [VOCl2(H2O)(C6H9O2)2] from powder diffraction data , 2002 .

[45]  K. Harris,et al.  Polymorphism of a novel sodium ion channel blocker. , 2003, Journal of pharmaceutical sciences.

[46]  Kenneth D. M. Harris,et al.  PowderSolve – a complete package for crystal structure solution from powder diffraction patterns , 1999 .

[47]  Roy L. Johnston,et al.  Implementation of Lamarckian concepts in a Genetic Algorithm for structure solution from powder diffraction data , 2000 .

[48]  Abraham Clearfield,et al.  Application of X-ray Powder Diffraction Techniques to the Solution of Unknown Crystal Structures , 1997 .