Service Center X-ray Diffraction

Tasks and goals of the service center

The Service Center X-ray diffraction offers single crystal and powder X-ray diffraction experiments as central service. It is included into research and teaching in the chemistry department and adjacent disciplines. It supplys the necessary databases and programs needed for the data evaluation and representation.

 

► Single crystal X-ray diffraction

Employee Service Center X-ray Diffraction - single crystal X-ray diffraction

Dr. Bernd Morgenstern
Campus C4.1
Room 3.01
Tel.: ++49/ 681/ 302-64073
E-Mail

 

 

With the establishment of the Service Center for X-ray Diffraction, the possibility to conduct single crystal X-ray diffraction experiments is now possible as central service for all groups on campus, surrounding research centers and in the industry.

This method allows the determination of the (molecular) solid state structure for the position and realtive arrangement of the individual atoms. For this, diffraction patterns of the crystal are recorded, from which the electron distribution can be extracted via Fourier synthesis.

Via this technique, the unambiguous proof the spacial atomic arrangement can be conducted, given a suitable single crystal exists.

Possibilities

The service offered ranges from the selection of suitable single crystals to the recording of a data set to the evaluation of the data along with the representation if the data as tables and drawings for publication.

Two single crystal X-ray diffractometers are available in the Service Center. An older Bruker X8 ApexII with CCD detector and a newer Bruker D8 Venture with a micro focus source for both Mo- and Cu-radiation. The more efficient X-ray source along with an advanced detector technology enables a rapid data acquisition and the measurement of significantly smaller single crystals. The permanent availability of Cu-radiation allows a determination if the "absolute configuration" of enantiomeric pure organic compounds. Both instruments are equipped with a cryogenic device for structure detemination down to 100 K

The quality of the data set and the linked quality of the structure solution and refinement are not only tied to the instrument but also significantly to the grade of the selected crystal. Enhancing the crystals quality during the crystallization step will be rewarded. However, since both instruments are equipped with area detectors, the tolerance with respect to lower quality crystals is enhanced. Therefore a preliminary structure determination is even possible on these specimens with the results, however, not being publishable.

An up to date license for the Cambridge Structural Database is available and allows the comparison of collected data with published results as well as statistical data evaluation.

Structure determination of biomolecules (protein crystallography) is not possible in the Service Center.

► Powder X-ray diffraction

Employee Service Center X-ray Diffraction - powder X-ray diffraction

Dr. Oliver Janka
Campus C4.1
Room 4.01
Tel.: ++49/ 681/ 302-70665
E-Mail

 

 

Powder X-ray diffraction allows for a non-destructive investigation of (usually) crystalline samples. With its help, the purity of the sample or the present phases (phase analysis) along with lattice parameters of the identified and refined compounds can be evaluated. If a sample contains more than one phase, the respective ratios can be determined via Rietveld refinement. Besides plain phase analysis, also a microstructure analysis (crystallite size, texture, strain) can be carried out. In case of a known crystal structure, besides the lattice parameters also the atomic positions and the isotropic thermal displacement parameters can be determined. Finally, temperature dependent measurements allow the characterization of e.g. structural phase transitions.

Measurements

The Service Center supports the planning of measurements, conducts them, including sample preparation and also performs a full refinement of the measurement data. A briefing for independent use of the instruments is possible if an increased use is anticipated.

Infrastructure

Currently, four powder diffractometers are available, all equipped with a copper source. Besides the Bruker D8 ADVANCE diffractometer, which is usually used for standard measurement requests, also three PANalytical X‘Pert Pro instruments are available. One of these is equipped with a high-temperature chamber from mri (temperature range 300-1273 K) and one is equipped with a 15-sample auto-changer. The latter can be used by persons with independent measurement rights.

Sensitive samples can be measured by using a “dome” or in sealed capillaries. With the help of a reaction chamber (Anton Paar XRK 900), measurements can be conducted under different gas atmospheres (Ar, N2, O2), at elevated pressures (10 bar) or in dynamic vacuum.

Bruker D8 ADVANCE Diffractometer

  • Bragg-Brentano geometry, measuring range 2θ ca. 3,5-150°
  • Cu radiation (40 kV, 40 mA)
  • detector: Lynxeye 1D
  • primary beam path: variable divergence slits, Ni filter, soller collimator
  • secondary beam path: variable divergence slits, soller collimator
  • auto sampler (6 racks each 15 samples)
  • other equipment: Anton Paar high-temperature oven chamber HTK1200N (300-1473 K, 1 bar), Anton Paar reactor chamber XRK900 (300-1173 K, 10 bar), capillary sample holder
 

PANalytical X‘Pert Pro – Instrument 1

  • Bragg-Brentano geometry, measuring range 2θ ca. 5-150°
  • Cu radiation (40 kV, 40 mA)
  • detector: PIXcel1D
  • primary beam path: soller collimator (horizontal, 0,02 o. 0,04 rad), variable divergence slit
  • secondary beam path: soller collimator (horizontal, 0,02 o. 0,04 rad), variable anti-scatter slit
  • auto sampler (1 racks each 15 samples)
  • other equipment: mirror and double monochromator
 

PANalytical X‘Pert Pro-MPD – Instrument 2

  • Bragg-Brentano geometry, measuring range 2θ ca. 5-150°
  • Cu radiation (40 kV, 40 mA)
  • detector: PIXcel1D
  • primary beam path: soller collimator (horizontal, 0,02 o. 0,04 rad), variable divergence slit
  • secondary beam path: soller collimator (horizontal, 0,02 o. 0,04 rad), variable anti-scatter slit
  • other equipment: Anton Paar high-temperature oven chamber HTK1200N (300-1473 K, 1 bar) – not in use
 

PANalytical X‘Pert Pro-MPD – Instrument 3

  • Bragg-Brentano geometry, measuring range 2θ ca. 5-150°
  • Cu radiation (40 kV, 40 mA)
  • detectors: MiniProp (gas ionization detector) and X’Celerator
  • primary beam path: soller collimator (horizontal, 0,02 o. 0,04 rad), divergence slit
  • secondary beam path: soller collimator (horizontal, 0,02 o. 0,04 rad), anti-scatter slit
  • high-temperature oven chamber MRI TC radiation (300-1273 K) with direct and indirect sample heating in Pt or Al2O3 crucibles
  • other equipment: multi purpose stage, sample holder with Φ rotation
 

User regulations, measurement orders & process

User regulations

For all measurements performed in the X-ray diffraction service center, the new user regulations will apply from February 1st 2021.
These can be dowloaded here (version of January 27th 2021).

 

Measurement applications

As of February 1st 2021, a measurement application form must be filled out for measurements and submitted with the samples.
Form for single crystal diffraction measurements
Form for powder diffraction measurements

 

Measurement procedure

As far as possible, the samples are processed in the order in which they are received. However, the expertise of the operator decides on the specific sequence. Please clarify the measurement conditions in advance by e-mail.
single crystal X-ray diffraction: scxrd(at)uni-saarland.de
powder X-ray diffraction: pxrd(at)uni-saarland.de

 

Sample drop-off

Single crystal X-ray diffraction:
Samples can be dropped off in building C4.1, room 3.01. Please call beforehand and bring the completed measurement form.
Since only a small single crystal is needed, the sample quantity is usually small. However, a larger quantity of crystals should be available for selection, since the quality of the crystal is directly proportional to the result. Material that is not needed is returned.
It is advantageous to leave the crystals in the solution. In other words, condense only until crystals form and then deliver well sealed. Solvent molecules are often included in the lattice, which easily escape due to their weak bonding, which then leads to the disintegration of the crystals. In addition, impurities still in the solution can cause the crystals to stick to the vessel wall after the solvent has been completely removed. As a result, they can no longer be removed undamaged. The size of the vessel should be in reasonably rational proportion to the amount of sample. It is no pleasure to fish out a few tiny crystals from a large flask, which are then still sitting almost unreachably on the side of the wall.
There are special procedures for substances that are sensitive to air and moisture. The procedure is agreed on a case-by-case basis.

Powder diffraction:
Samples can be dropped off in building C4.1, room 4.01. Please make an appointment in advance and bring the measurement application form completely filled out.
The required sample quantity depends on the substance class and the desired measurement method. Details will be clarified in the preliminary discussion.
There are special procedures for substances that are sensitive to air and moisture. Here, too, the procedure will be discussed on a case-by-case basis.

Publications

In the case of publications, the contributions of the service center are to be considered according to scientific practice. All manuscripts containing X-ray powder data measured at the Service Center must be submitted for review. In this way, factual errors related to the presentation of the data can be avoided. Figures as well as a crystallographic summary (cif file - Crystallographic Information File) will be provided.
Successful publications or patents based on results of the services provided must be communicated to the responsible persons of the service center.

Text blocks for powder X-ray diffraction experiments - PDF - docx

► Further information and services

Lectures at Saarland University

The following lectures and classes focus (partially) on X-ray diffraction:

  • Festkörperchemie und Strukturchemie (solid state and structural chemistry, AC05), winter term, held by Prof. Kickelbick and Dr. Janka
  • Strukturchemie und Kristallographie (structural chemistry and crystallography, AC10), winter term, held by Prof. Kickelbick and Dr. Janka
  • Praktikum Kristallographie und Strukturchemie (lab class: crystallography and structural chemistry, ACK), winter term, held by Dr. Janka

Databases and programs

The service center for X-ray diffraction offers access to the CSD (The Cambridge Structural Database) and the ICSD (Inorganic Crystal Structure Database). In these, structural data of organic and metal-organic or coordination compounds and inorganic (solid state) compounds are deposited. In addition a powder diffraction database (PDF-2) is available.
For graphical representation and structural investigations, acces to the programs Diamond, Mercury and Platon is available.

 

Publications with contributions of the service center

2022

37

T. I. Demirer, B. Morgenstern, D. M. Andrada:
Synthesis, Structure, and Bonding Analysis of Lewis Base and Lewis Acid/Base-Stabilized Phosphanylgallanes
Eur. J. Inorg. Chem. 2022, e202200477.
[DOI:org/10.1002/ejic.202200477]

36

M. Hunsicker, N. E. Poitiers, V. Huch, B. Morgenstern, M. Zimmer, D. Scheschkewitz:
Interlinkage of a siliconoid with a silsesquioxane: en route to a molecular model system for silicon monoxide
Z. Anorg. Allg. Chem. 2022, 648, e202200239.
[DOI:org/10.1002/zaac.202200239]

35

I.-A. Bischoff, B. Morgenstern, A. Schäfer:
Heavier N-heterocyclic half-sandwich tetrylenes
ChemComm. 2022, d2cc03107h.
[DOI:org/10.1039/D2CC03107H]

34

A. Koner, B. Morgenstern, D. M. Andrada:
Metathesis Reactions of a NHC-Stabilized Phosphaborene
Angew. Chem. Int. Ed. 2022, 61,e202203345.
[https://doi.org/10.1002/anie.202203345]

33

W. Hofer, E. Oueis, A. A. Fayad, F. Deschner, A. Andreas, L. P. de Carvalho, S. Hüttel, S. Bernecker, L. Pätzold, B. Morgenstern, N. Zaburannyi, M. Bischoff, M. Stadler, J. Held, J. Herrmann, R. Müller:
Regio- and Stereoselective Epoxidation and Acidic Epoxide Opening of Antibacterial and Antiplasmodial Chlorotonils Yield Highly Potent Derivatives
Angew. Chem. Int. Ed. 2022, 61,e202202816.
[DOI:org/10.1002/anie.202202816]

32

N. E. Poitiers, V. Huch, B. Morgenstern, M. Zimmer, D. Scheschkewitz:
Siliconoid Expansion by a Single Germanium Atom through Isolated Intermediates
Angew. Chem. Int. Ed. 2022, 61,e202205399.
[DOI:org/10.1002/anie.202205399]

31

A. Grünewald, B. Goswami, K. Breitwieser, B. Morgenstern, M. Gimferrer, F. W. Heinemann, D. M. Momper, C. W. M. Kay, D. Munz:
Palladium Terminal Imido Complexes with Nitrene Character
J. Am. Chem. Soc. 2022, 144, 8897-8901.
[DOI:org/10.1021/jacs.2c02818]

30

M. Lambert, N. E. Poitiers, V. Huch, A. Goforth, D. Scheschkewitz:
Silicon-carbon hybrid [2]-ladderanes
Z. Anorg. Allg. Chem. 2022, 648, e202200030.
[DOI: org/10.1002/zaac.202200030]

29

L. H. Staub, J. Lambert, C. Müller, B. Morgenstern, M. Zimmer, J. Warken, A. Koldemir, T. Block, R. Pöttgen, A. Schäfer:
Bis(di-tert-butylindenyl)tetrelocenes
Dalton Transactions  2022, 51, 10714-10720.
[DOI: org/10.1039/d2dt00582d]

28

N. Bachmann, L. Wirtz, B. Morgenstern, C. Müller, A. Schäfer:
Crystal structure of 1,1‘, 2,2‘, 4,4‘-hexaisopropylmagenesocene
Acta Crystallographica 2022, E78, 287-290.
[DOI:org/10.1107/S2056989022001189]

27

I.-A. Bischoff, B. Morgenstern, A. Schäfer:
Synthesis and structure of an asymmetrical sila[1] magnesocenophane
Z. Naturforsch. 2022, B77, 95-98.
[DOI:org/10.1515/znb-2021-0152]

26

W. Haider, M. D. Calvin-Brown, I.-A. Bischoff, V. Huch, B. Morgenstern, C. Müller, T. Sergeieva, D. M. Andrada, A. Schäfer:
Diarylpnictogenyldialkylalanes-Synthesis, structures, Bonding Analysis, and CO2 Capture
Inorg. Chem. 2022, 61, 1672-1684.
[DOI:org/10.1021/acs.inorgchem.1c03494]

25

 

S. Baur, K. Brix, A. Feuerstein, O. Janka, R. Kautenburger:
Retention of waste cocktail elements onto characterised calcium silicate hydrate (C–S–H) phases: A kinetic study under highly saline and hyperalkaline conditions
Appl. Geochem. 2022, accepted.
[DOI: 10.1016/j.apgeochem.2022.105319]

24

 

S. Engel, J. Bönnighausen, F. Stegemann, R. S. Touzani, O. Janka:
SrAl5Pt3 and Sr2Al16Pt9 – two new strontium aluminum platinides
Z. Naturforsch B. 2022, accepted.
[DOI: 10.1515/znb-2022-0012]

2021

23

D. Elenkova, R. Lyapchev, J. Romanova, B. Morgenstern, Y. Dimitrova, D. Dimov, M. Tsvetkov, J. Zaharieva:
Luminescent Complexes of Europium (III) with 2-(Phenylethynyl)-1,10-phenanthroline: The Role of the Counterions
Molecules 2021, 26, 7272.

[DOI:org/10.3390/molecules26237272]

 

22

 

A. K. Boehm, S. Husmann, M. Besch, O. Janka, V. Presser, M. Gallei:
Porous Mixed-Metal Oxide Li-Ion Battery Electrodes by Shear-Induced Co-assembly of Precursors and Tailored Polymer Particles
ACS Appl. Mater. Interfaces 2021, 13, 61166-61179.

[DOI: 10.1021/acsami.1c19027]

21

 

J.-F. Kannengießer, M. Briesenick, D. Meier, V. Huch, B. Morgenstern, G. Kickelbick:
Synthesis and Hydrogen-Bond Patterns of Aryl-Group Substituted Silanediols and -triols from Alkoxy- and Chlorosilanes
Chem. Eur. J. 2021, 27, 16461-16476.

[DOI: 10.1002/chem.202102729]

20

 

L. Wirtz, J. Lambert, B. Morgenstern, A. Schäfer:
Cross-Dehydrocoupling of Amines and Silanes Catalyzed by Magnesocenophanes
Organometallics2021, 40, 2108-2117.

[DOI: 10.1021/acs.organomet.1c00245]

19

 

A. Koner, T. Sergeieva, B. Morgenstern, D. M. Andrada:
A Cyclic Iminoborane-NHC Adduct: Synthesis, Reactivity, and Bonding Analysis
Inorg. Chem. 2021, 60, 14202-14211.

[DOI: 10.1021/acs.inorgchem.1c01583]

18

 

P. K. Majhi, M. Zimmer, B. Morgenstern, V. Huch, D. Scheschkewitz:
Transition Metal Complexes of Heavier Vinylidenes: Allylic Coordination vs Vinylidene-Alkyne Rearrangement at Nickel
J. Am. Chem. Soc. 2021, 143, 13350-13357.

[DOI: 10.1021/jacs.1c06453]

17

 

P. K. Majhi, M. Zimmer, B. Morgenstern, D. Scheschkewitz:
Transition-Metal Complexes of Heavier Cyclopropenes: Non-Dewar-Chatt-Duncanson Coordination and Facile Si=Ge Functionalization
J. Am. Chem. Soc.2021, 143, 8981-8986.

[DOI: 10.1021/jacs.1c04419]

16

 

T. Büttner, K. Weisshaar, P. Willmes, V. Huch, B. Morgenstern, R. Hempelmann, D. Scheschkewitz:
Synthesis and electrochemistry of remotely thioether-functionalized disilenes
Z. Anorg. Allgem. Chem. 2021, 647, 1674-1678.

[DOI: 10.1002/zaac.202100161]

15

 

L. Klemmer, A.-L. Thömmes, M. Zimmer, V. Huch, B. Morgenstern, D. Scheschkewitz:
Metathesis of Ge=Ge double bonds
Nature Chem. 2021, 13, 373-377.

[DOI: 10.1038/s41557-021-00639-9]

14

 

M. Veith, F. Sahin, S. Nadig, V. Huch, B. Morgenstern:
Transformations of the polycyclic Alumosiloxane Al2(OSiPh2OSiPh2O)3 into new Polycycles and Co(II) and In(III) derivatives of (Ph2SiO)8[Al(O)OH]4
Z. Anorg. Allg. Chem. 2021, 647, 1709-1720.

[DOI: 10.1002/zaac.202100126]

13

 

P. Pinter, C. M. Schüßlbauer, F. A. Watt, N. Dickmann, R. Herbst-Irmer, B. Morgenstern, A. Grünwald, T. Ullrich, M. Zimmer, S. Hohloch, D. M. Guldi, D. Munz:
Bright luminescent lithium and magnesium carbene complexes
Chem. Sci. 2021, 12, 7401-7410.

[DOI: 10.1039/D1SC00846C]

12

 

C. Müller, J. Warken, V. Huch, B. Morgenstern, I.-A. Bischoff, M. Zimmer, A. Schäfer:
Diphosphanylmetallocenes of Main-Group Elements
Chem. Eur. J.2021, 27, 5600-6510.

[DOI: 10.1002/chem.202005198]

11

 

S. Lauk, M. Zimmer, B. Morgenstern, V. Huch, C. Müller, H. Sitzmann, A. Schäfer:
Tetra- and Pentaisopropylcyclopentadienyl Complexes of Group 15 Elements
Organometallics2021, 40, 618- 626.

[DOI: 10.1021/acs.organomet.1c00008]

10

 

A. T. Kell, N. M. Obeid, P. Bag, M. Zimmer, V. Huch, D. Scheschkewitz:
Reactivity of Phenylacetylene toward Unsymmetrical Disilines: Regiodivergent [2+2] Cycloaddition vs. CH Addition
Z. Anorg. Allg. Chem. 2021, 647, 1751-1758.

[DOI: 10.1002/zaac.202100137]

9

 

T. Stemler, C. Hoffmann, I. M. Hierlmeier, S. Maus, E. Krause, S. Ezziddin, G. Jung, M. D. Bartholomä:
A Structure-Activity Relationship Stucy of Bimodal BODIPY-Labeled PSMA-Targeting Biconjugates
ChemMedChem2021, 16, 2535-2545.

[DOI: 10.1002/cmdc.202100210]

8

 

P. K. Majhi, V. Huch, D. Scheschkewitz:
A Mixed Heavier Si=Ge Analoque of a Vinyl Anion
Angew. Chem. Int. Ed. 2021, 60, 242-246.

[DOI: 10.1002/anie.202009406]

7

 

W. Cao, S. Yin, M. Bitsch, S. Liang, M. Plank, M. Opel, M. A. Scheel, M. Gallei, O. Janka, M. Schwartzkopf, S. V. Roth, P. Müller-Buschbaum:
In Situ Study of FePt Nanoparticles-Induced Morphology Development during Printing of Magnetic Hybrid Diblock Copolymer Films
Adv. Funct. Mater. 2021, 32, 2107667.

[DOI: 10.1002/adfm.202107667]

6

 

E. Gießelmann, R. S. Touzani, B. Morgenstern, O. Janka:
Synthesis, crystal and electronic structure of CaNi2Al8
Z. Naturforsch B 2021, 76b, 659-668.

[DOI: 10.1515/znb-2021-0105]

5

 

B. Oberhausen, G. Kickelbick:
Induction heating induced self-healing of nanocomposites based on surface-functionalized cationic iron oxide particles and polyelectrolytes
Nanoscale Adv. 2021, accepted.

[DOI: 10.1039/D1NA00417D]

4

 

D. Meier, V. Huch, G. Kickelbick:
Aryl-group substituted polysiloxanes with high-optical transmission, thermal stability, and refractive index
J. Polym. Sci. 2021, accepted.

[DOI: 10.1002/pol.20210316]

3

 

l. Wang, K. Frisella, P. Srimuk, O. Janka, G. Kickelbick, V. Presser:
Electrochemical lithium recovery with lithium iron phosphate: What causes performance degradation and how can we improve the stability?
Sustain. Energy Fuels 2021, 3124-3133.

[DOI: 10.1039/D1SE00450F]

2

 

S. Pohl, O. Janka, E. Füglein, G. Kickelbick:
Thermoplastic Silsesquioxane Hybrid Polymers with a Local Ladder-Type Structure
Macromolecules 2021, 54, 3873-3885.

[DOI: 10.1021/acs.macromol.1c00310]

1

 

P. Shankhari, O. Janka, R. Pöttgen,B. P. T. Fokwa:
Rare-Earth-free Magnets: Enhancing Magnetic Anisotropy and Spin Exchange Toward High-TC Hf2MIr5B2(M = Mn, Fe)
J. Am. Chem. Soc. 2021, 4205-4212.

[DOI: 10.1021/jacs.0c10778]