Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector

A specialized quantum area detector for electron diffraction studies makes it possible to solve the structure of small organic compound nanocrystals in non-cryo conditions by direct methods.

[1]  R. Horisberger,et al.  A pixel detector for the protein crystallography beamline at the SLS , 2002 .

[2]  U. W. Arndt,et al.  The Rotation method in crystallography : data collection from macromolecular crystals , 1977 .

[3]  Tamir Gonen,et al.  High-resolution structure determination by continuous rotation data collection in MicroED , 2014, Nature Methods.

[4]  David B. Williams,et al.  Transmission Electron Microscopy , 1996 .

[5]  B. van der Heijden,et al.  A Gigabit per second read-out system for Medipix Quads , 2011 .

[6]  G. Sheldrick SHELXT – Integrated space-group and crystal-structure determination , 2015, Acta crystallographica. Section A, Foundations and advances.

[7]  C. Scheringer,et al.  Nicotinic acid, C6H5NO2: refinement , 1983 .

[8]  U. Kolb,et al.  Towards automated diffraction tomography: part I--data acquisition. , 2007, Ultramicroscopy.

[9]  Jan Pieter Abrahams,et al.  A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals , 2013, Acta crystallographica. Section D, Biological crystallography.

[10]  Mauro Gemmi,et al.  Fast electron diffraction tomography , 2015 .

[11]  Sven Hovmöller,et al.  Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders , 2015, IUCrJ.

[12]  P. Andrew Karplus,et al.  Linking Crystallographic Model and Data Quality , 2012, Science.

[13]  A. Ikni,et al.  Electron Properties of Carbamazepine Drug in Form III , 2013 .

[14]  J. Abrahams,et al.  Evaluation of Medipix2 detector for recording electron diffraction data in low dose conditions , 2011 .

[15]  Lianmao Peng ELECTRON ATOMIC SCATTERING FACTORS AND SCATTERING POTENTIALS OF CRYSTALS , 1999 .

[16]  R. Henderson The potential and limitations of neutrons, electrons and X-rays for atomic resolution microscopy of unstained biological molecules , 1995, Quarterly Reviews of Biophysics.

[17]  R. Henderson,et al.  Detective quantum efficiency of electron area detectors in electron microscopy , 2009, Ultramicroscopy.

[18]  G. G. Stokes "J." , 1890, The New Yale Book of Quotations.

[19]  Andreas F. M. Kilbinger,et al.  Ab-initio crystal structure analysis and refinement approaches of oligo p-benzamides based on electron diffraction data. , 2012, Acta crystallographica. Section B, Structural science.

[20]  George M. Sheldrick,et al.  ShelXle: a Qt graphical user interface for SHELXL , 2011, Journal of applied crystallography.

[21]  David B. Williams,et al.  Transmission Electron Microscopy: A Textbook for Materials Science , 1996 .

[22]  G. Sheldrick A short history of SHELX. , 2008, Acta crystallographica. Section A, Foundations of crystallography.

[23]  C. Giacovazzo,et al.  Crystal structure determination and refinement via SIR2014 , 2015 .

[24]  Andrea Thorn,et al.  Enhanced rigid-bond restraints , 2012, Acta Crystallographica Section A: Foundations of Crystallography.

[25]  M. Gemmi,et al.  Scanning reciprocal space for solving unknown structures: energy filtered diffraction tomography and rotation diffraction tomography methods , 2012 .

[26]  U. Kolb,et al.  Structural Characterization of Organics Using Manual and Automated Electron Diffraction , 2010 .

[27]  Sven Hovmöller,et al.  Three-dimensional rotation electron diffraction: software RED for automated data collection and data processing , 2013, Journal of applied crystallography.

[28]  R. Dinapoli,et al.  Medipix2: A 64-k pixel readout chip with 55-/spl mu/m square elements working in single photon counting mode , 2001 .

[29]  Rafael Ballabriga,et al.  Timepix, a 65k programmable pixel readout chip for arrival time, energy and/or photon counting measurements , 2007 .

[30]  U. Kolb,et al.  Towards automated diffraction tomography. Part II--Cell parameter determination. , 2008, Ultramicroscopy.

[31]  M. Eddleston,et al.  Transmission electron microscopy of pharmaceutical materials. , 2010, Journal of pharmaceutical sciences.

[32]  Randy J. Read,et al.  Overview of the CCP4 suite and current developments , 2011, Acta crystallographica. Section D, Biological crystallography.

[33]  U. Kolb,et al.  "Ab initio" structure solution from electron diffraction data obtained by a combination of automated diffraction tomography and precession technique. , 2009, Ultramicroscopy.

[34]  Tim Gruene,et al.  New method to compute Rcomplete enables maximum likelihood refinement for small datasets , 2015, Proceedings of the National Academy of Sciences.

[35]  U. Kolb,et al.  Automated electron diffraction tomography – a new tool for nano crystal structure analysis , 2011 .