Properties of an electron-density map derived from a limited number of experimentally determined triplet phases.

In a previous communication [Weckert et al. (1999). Acta Cryst. D55, 1320-1328], the feasibility of the measurement of a large set of triplet phases by three-beam interference was demonstrated. This paper reports the methodology for the calculation of an electron-density map from this limited amount of experimental phase information and the map's properties with respect to model building and refinement. The tetragonal form of hen egg-white lysozyme (HEWL) was chosen as a test structure for the development of this method. The quality of the electron-density map obtained from all measured triplet phases allows a straightforward and nearly complete interpretation. The starting model was refined to a final R value of 17.4%. In a second step, the minimum number of phased reflections needed for the interpretation of an electron-density map was investigated, applying criteria based on |F| and resolution.

[1]  Rex A. Palmer,et al.  Structure determination by X-ray crystallography , 1977 .

[2]  A. Brunger Free R value: a novel statistical quantity for assessing the accuracy of crystal structures. , 1992 .

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

[4]  E. G. Sherry,et al.  STRUCTURE DETERMINATION I , 1960 .

[5]  P. Main On the application of phase relationships to complex structures. XI. A theory of magic integers , 1977 .

[6]  King,et al.  Direct phase determination of large macromolecular crystals using three-beam x-ray interference. , 1991, Physical review letters.

[7]  E. Weckert,et al.  A feasibility study of experimental triplet-phase determination in small proteins. , 1991, Acta crystallographica. Section A, Foundations of crystallography.

[8]  E. Weckert,et al.  Multiple-Beam X-ray Diffraction for Physical Determination of Reflection Phases and its Applications , 1997 .

[9]  P. Main On the application of phase relationships to complex structures. XII. The use of magic integers in phase determination , 1978 .

[10]  M. Woolfson,et al.  The application of phase relationships to complex structures. VlI. Magic integers , 1975 .

[11]  D. McRee Practical Protein Crystallography , 1993 .

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

[13]  David Blow,et al.  Direct Methods In Crystallography , 1962 .