The SMS laboratory possesses the X-ray diffraction devices listed hereafter (click on the links to know more):
 
 
 
 
 
 
 
 
 

 

 

 

 

 

 

Powder X-ray diffraction

 

  •  The D8 Discover diffractometer with a -theta/-theta geometry In-SituX®

  

Supplier: Bruker AXS         

Principle: The -theta/-theta geometry (inverted Bragg-Brentano geometry) of this apparatus permits in-situ analysis of solid phase in suspension in a liquid phase (reactor capacity is 100 mL), or solid phase in equilibrium with its vapor.

Type of analyses performed: This aparatus is suited for in-situ monitoring of solution crystallization processes: the reactor temperature (from -30 to 70 °C) and solvent injection are controlled during the process et the system analyzes the nature of the solid phase in suspension. This allows for instance to determine temperatures of phase transition or peritectic temperatures (solvation, desolvation). In a nutshell, detection of efflorescent solvates is made easy with In-SituX.

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Highlights:

- Neurohr, C.; Marchivie, M.; Lecompte, S.; Cartigny, Y.; Couvrat, N.; Sanselme, M.; Subra-Paternault, P. Naproxen−Nicotinamide Cocrystals: Racemic and Conglomerate Structures Generated by CO2 Antisolvent Crystallization Cryst. Growth Des. 2015, 15, 4616-4626.
- Lafontaine, A.; Sanselme, M.; Cartigny, Y.; Cardinaël, P.; Coquerel, G. Characterization of the transition between the monohydrate and the anhydrous citric acid J. Therm. Anal. Calorim. 2013, 112, 307-315.
- Coquerel, G.; Sanselme, M.; Lafontaine, A. WO2012/136921 A1, 2012
 
 
 
 
  • The D8 Discover Diffractometer

      

Supplier: Bruker AXS         

Principle: X-ray diffraction analyses (in reflexion mode / Bragg-Brentano geometry) of powdered samples. The sample holder is equipped with a spinner than reduces texture and preferiental orientation effects.

Type of analyses performed: This device is dedicated to routine analyses and enables the obtention of good quality diffractograms in less than 10 minutes. The sample holder can also be equipped with a cooling system.
 
 
 
  •  D5005 Diffractometer     

      

Supplier: Bruker AXS         

Principle: X-ray powder diffraction analysis of crystalline samples in theta theta geometry (Bragg Brentano geometry). The sample holder can be thermostated with a TTK450 Anton Parr chamber (temperature range: -30 up to 200 °C). This system is equipped with a copper anode, Ni filter, and scintillator detector.

Type of analyses performed: This device allows to follow the evolution of the crystalline phase according to the temperature, and therefore to determine, for examples, the temperature transition of a solid solid transition or of a desolvation process. Therefore, these data are of main interest for the construction of a phase diagram

Highlights:

- Renou L., Coste S., Cartigny Y., Petit M.-N., Vincent C., Schneider J.-M., Coquerel G. Mechanism of hydration and dehydration of ciclopirox olamine (1:1) Cryst. Growth Des. 2009, 9, 3918-3927.
- Neurohr, C.; Marchivie, M.; Lecompte, S.; Cartigny, Y.; Couvrat, N.; Sanselme, M.; Subra-Paternault, P. Naproxen−Nicotinamide Cocrystals: Racemic and Conglomerate Structures Generated by CO2 Antisolvent Crystallization Cryst. Growth Des. 2015, 15, 4616-4626.
 
 
 
  •  Equinox 100 benchtop diffractometer    

     

Supplier: INEL                      

Principle: X-ray powder diffraction analysis of crystalline samples (asymmetrical reflexion geometry). The system is equipped with copper anode, and curved detector that allows to analyse on a large range on 2theta in one “shoot” (from 3° up  to 110°).

Type of analyses performed: This apparatus allows the routine anlysis of crystalline powder sample, and can also be equipped with a 6 position sample holder.

 
 
 

Single Crystal X-ray diffraction

  •  D8 Smart Diffractometer   

Supplier: INEL                     

Principle: Single crystal diffraction analysis to achieve the structural resolution of crystalline solid.

Type of analyses performed: The system is equipped with a temperature regulator that allows the data to be recorded at low temperature (from room temperature down to -100°C).

Highlights:

- Structural studies of several solvated potassium salts of tenetoprazole crystallizing as conglomerates. Tauvel G., Sanselme M., Coste-LecomteS., Petit S., Coquerel G. J. Mol. Struct. 2009, 936, 60-66
- Physical transformations of the active pharmaceutical ingredient BN83495: enantiotropic and monotropic relationships. Access to several polymorphic form by using various solvation-desolvation processes. D. Martins, M. Sanselme, O. Houssin, V. Dupray, M.N. Petit, D. Pasquier, C. Diolez and G. Coquerel. CrystEngComm, 2012, 14 (7), 2507 - 2519, (Special issue on pharmaceuticals)
- Detection of order-disorder transition in organic solids by using Temperature Resolved Second Harmonic Generation (TR-SHG). S. Clevers, C. Rougeot, F. Simon, M. Sanselme, V Dupray, G. Coquerel. J. Mol. Structure, 2014, 1078, 61–67
- Access to single crystals of (±)-Form IV of Modafinil by crystallization in gels; comparisons between (±)-Forms I, III and IV and (-)-Form I. J. Maheux, M. Sanselme and G. Coquerel. Crystal Growth and Design, 2013, 13 (2), pp 908-917