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29.06.2011 1
Tatiana E.Gorelik, Galina Matveeva, Ute Kolb
Institute of Physical Chemistry,Johannes-Gutenberg University
Mainz, Germany
APPLICATION OFAUTOMATED ELECTRON DIFFRACTION
TO STRUCTURAL INVESTIGATIONOF MOLECULAR CRYSTALS
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Transmission electron microscope (TEM) Imaging High-resolution imaging
Elemental analysis (EDX)
Electron diffraction
APPLICATION OF AUTOMATED ELECTRON DIFFRACTION TO STRUCTURAL INVESTIGATION OF MOLECULAR CRYSTALS
APPLICATION OF AUTOMATED ELECTRON DIFFRACTION TO STRUCTURAL INVESTIGATION OF MOLECULAR CRYSTALS
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Single crystal electron diffraction: tilt seriesPowder electron diffraction
Pawley and Rietveldrefinements using electrondiffraction from L12-typeintermetallic Au3Fe1-xnanocrystals duringtheir in-situorder–disorder transition
Zhiping Luo, YolandaVasquez, James F.Bondi,Raymond E.Schaak
Ultramicroscopy, 2011
APPLICATION OF AUTOMATED ELECTRON DIFFRACTION TO STRUCTURAL INVESTIGATION OF MOLECULAR CRYSTALS
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Single crystal electron diffraction: tilt seriesPowder electron diffraction
Pawley and Rietveldrefinements using electrondiffraction from L12-typeintermetallic Au3Fe1-xnanocrystals duringtheir in-situorder–disorder transition
Zhiping Luo, YolandaVasquez, James F.Bondi,Raymond E.Schaak
Ultramicroscopy, 2011
Structure solution using zonal electron diffraction data: historical overview
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Rigamonti, R., La struttura della catena paraffinica studiata mediante i raggi dielettroni, Gazzetta Chimica Italiana 66 174-182 (1936)
D.L. Dorset, Structural electron crystallography, Plenum New York (1995)
Voigt-Martin et al., The use of simulation mehods to obtain the structure andconformation of 10-cyano-9,9‘-bianthryl by electron diffraction and high-resolution imaging, Ultramicrocopy 57, 29-43 (1995)
Organic samples
Biological samples2D Protein crystals
Dorset, D.L., Direct structure analysis in protein electron crystallography:crystallographic phases for halorhodopsin to 6Å resolution, Proc Natl Acad SciUSA 92(22), 10074–10078 (1995)
Weirich et al. A crystal structure determined with 0.02 Å accuracy with electronmicroscopy, Nature 382, 144 (1996)
Hovmöller et al., Accurate atomic positions from electron microscopy, Nature311, 238-241 (1984)
Inorganic samples(thin)
→ Solution using structure factor phases derived from HRTEMKühlbrandt, W. et al. Atomic model of plant-light harvesting complex by electroncrystallography, Nature 367, 614, (1997) – 3.4 Å resolution
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Automated electron Diffraction Tomography (ADT):collection of the complete reciprocal data rather than zonal patterns
AUTOMATED ELECTRON DIFFRACTION: THE EXPERIMENT
Towards automated diffraction tomography. Part I - Data AcquisitionU. Kolb, T. Gorelik, C. Kubel, M.T. Otten and D. Hubert,Ultramicroscopy, 107, 507-513 (2007).
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AUTOMATED ELECTRON DIFFRACTION: DATA PROCESSING
Automated electron Diffraction Tomography (ADT):collection of the complete reciprocal data rather than zonal patterns
Towards automated diffraction tomography. Part II - cell parameter determinationU. Kolb, T. Gorelik, M.T. Otten, Ultramicroscopy, 108, 763-772 (2008).
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AUTOMATED ELECTRON DIFFRACTION: DATA PROCESSING
Automated electron Diffraction Tomography (ADT):collection of the complete reciprocal data rather than zonal patterns
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Minerals:Mullite Al6Si2O13
SarrabusiteCharoite-96Charoite-90
Intermetallicnanophases:ZnSb, Zn8Sb7
Ca-compounds:Calcite, Vaterite
Calcium silicate hydrateCa5Si6O17·5H2O
Metal OrganicFrameworks (MOF):
MUF-4lBasolite
High pressure phases:HP hydrous Al-pyroxene
(Mg2Al(OH)2AlSiO6)
Organic-inorganichybrids:
ECS3, ECS5
Organic:NLO-active material
Organic pigmentsAmides
Zeolites:ZSM-5 (NaxAlxSi96-xO192)
Natrolite Na2Al2Si3O10·2H2OIM-5
RKL 040
Phosphates:SrP3N5O
Ba6Br3P12N17O9
Oxides:Na2W4O13Li2Ti3NiO8
NaHTi3O7·H2ONa2Ti6O13
MORE THAN 30 STRUCTURES ARE SOLVED FROM ADT DATA BY NOW (16 OUT OF THEM - NEW)
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agglomeratedcrystalsZn8Sb7 ~40 nm
AUTOMATED ELECTRON DIFFRACTION TOMOGRAPHY
small crystals radiation damage
disorder
200 nm
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Radiation damage: CNBA
STEM vs. TEM;Distribute the dose (crystal bending!);Cool the sample
e-dose rate:0.2-0.3 e/A2s
ELECTRON BEAM DAMAGE
STEM
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Orthorombic paracetamol (Pcab)
ADT As given byHaisa et al., 1974
11.4 A 11.805 A
17.4 A 17.164 A
7.6 A 7.393 A
90.1° 90°
90.0° 90°
88.1°* 90°
Projection (010):extinctions along c* direction(b-glide plane)
Material provided by Elena Boldyreva,Novosibirsk State University
ADT: UNIL CELL PARAMETERS DETERMINATION
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Orthorombic paracetamol (Pcab)
ADT As given byHaisa et al., 1974
11.4 A 11.805 A
17.4 A 17.164 A
7.6 A 7.393 A
90.1° 90°
90.0° 90°
88.1°* 90°
Projection (010):extinctions along c* direction(b-glide plane)
Material provided by Elena Boldyreva,Novosibirsk State University
ADT: UNIL CELL PARAMETERS DETERMINATION
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ADT: STACKING FAULTS - DISORDER
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Conclusion
Caution during data acquisition
Lattice cell parameters determination is always possible …
Alternative structure solution approaches formedium-resolution data
Direct methods structure solution for high resolution data
APPLICATION OF AUTOMATED ELECTRON DIFFRACTION TO STRUCTURAL INVESTIGATION OF MOLECULAR CRYSTALS
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Group
Ute Kolb
Galina MatveevaEnrico MugnaioliAndrew StewartIryna Andrusenko
Sebastian SchlittUlrich Heil
Rudolf WurfelRobert Branscheid
Financial support SFB 625
Max Otten, FEI, Eindhoven, The NetherlandsJacco van de Streek, Avant-garde Materials Simulation, FreiburgMartin U. Schmidt, University of Frankfurt-am-MainAndreas F.M. Kilbinger, Institute of Organic Chemistry, Mainz