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Structure Determination by Powder Diffractometry Round Robin

Description of the Round Robin Samples

The SDPDRR Homepage is at http://www.cristal.org/SDPDRR/

In order to help you to decide which method will be necessary, here are the characteristics of both samples and all patterns (you may decide to cope with only one of them). All data was collected at room temperature :


Sample 1

[Co(NH3)5CO3]NO3.H2O

Kindly supplied by Zhu Jianghai, Center for Analysis &  Measurement Fudan University Shanghai.

  • Crystal system: monoclinic 
  • Cell : a = 7.673A, b = 9.628 A, c = 7.077 A, beta = 106.28° 
  • Space groups : P21/m or P21 
Patterns:
  • 3 conventional X-ray (Cu K-alpha) 
  • Bragg Brentano 
Pattern 1a) China - Highly packed sample 
(minimal FWHM ~ 0.12° 2-theta) 
  • Filename: Zhu1.*
  • Run on Rigaku D/max-B 
  • Rotating Anode Cu 
  • Wavelengths: 1.54056 and 1.54439 A 
  • Generator Power: 120mA, 40KV 
  • Goniometer Radius: 185mm 
  • Divergence Slit: 0.5°
  • Receiving Slit Aperture: 0.15mm 
  • Sollers Slit Acceptance Angle: 0.5° 
  • Diffracted Beam Monochromator: flat graphite crystal 
  • Start, Step, Stop: 10.06, 0.02, 120.04 
  • Counting time: 30sec/step 
  • Vertical Sample Holder: 20x20mm sample surface
  • No spinning
Pattern 1b) Le Mans - Side-loaded sample holder 
(minimal FWHM ~ 0.13° 2-theta) 
  • Filename: Zhu2.*
  • Run on Siemens D501 
  • Tube Type Siemens Cu FF
  • Wavelengths: 1.54056 and 1.54439 A 
  • Generator Power: 28mA, 38KV 
  • Goniometer Radius: 200.5mm 
  • Divergence Slit: 0.3° 
  • Receiving Slit Aperture: 0.05° 
  • Sollers Slit Acceptance Angle: 2°
  • Diffracted beam curved graphite monochromator
  • Start, Step, Stop: 10.00, 0.02, 130.04 
  • Counting time: 24 seconds per point 
  • Horizontal Sample Holder: 40 x 20mm sample surface 
  • No Spinning
Pattern 1c) Le Mans - Sample dusted through a sieve: free of preferred orientation (FWHM ~ 0.25° 2-theta) 
  • Filename: zhu3.*
  • Run on Siemens D501, 
  • Tube Type Siemens Cu FF
  • Wavelengths: 1.54056 and 1.54056 A 
  • Generator Power: 28mA, 38KV 
  • Goniometer Radius: 200.5mm 
  • Divergence Slit: 1° 
  • Receiving Slit Aperture: 0.15° 
  • Sollers Slit Acceptance Angle: 2°
  • Diffracted beam curved graphite monochromator
  • Start, Step, Stop: 10.00, 0.02, 119.68 
  • Counting time: 28 seconds per point. 
  • Horizontal Sample Holder: 40 x 20mm sample surface
  • No Spinning

Sample 2

C22H24N2O8HCl

Pharmaceutical :
From the Aldrich Chemical Company Inc.
Milwaukee, WI 53233 USA
Reference : 25,016-3     [64-75-5]
Tetracycline Hydrochloride 98%, 25g
Lot : TQ
No. : 14219PQ
For laboratory use only.

  • Crystal system: orthorhombic 
  • Cell : a = 10.981 A, b = 12.853 A,
    c = 15.733 A,
     
  • Space group : P212121 
Patterns:
  • Conventional X-ray (Cu K-alpha) - Bragg Brentano 
  • Capillary/Image-Plate system 
Pattern 2a) Le Mans - using a side-loaded sample holder (minimal FWHM ~ 0.15° 2-theta) 
  • Filename: aldxconv.*
  • Run on Siemens D501 
  • Tube Type Siemens Cu FF 
  • Wavelengths: 1.54056 and 1.54439 A 
  • Generator Power: 28mA, 38KV 
  • Goniometer Radius: 200.5mm 
  • Divergence Slit: 0.3° 
  • Receiving Slit Aperture: 0.05° 
  • Sollers Slit Acceptance Angle: 2° 
  • Diffracted beam curved graphite monochromator 
  • Start, Step, Stop: 10.06, 0.02, 120.04 
  • Counting time: 48 sec./point 
  • Horizontal Sample Holder: 40x20 mm sample surface
  • No Spinning
Pattern 2b) Daresbury - Beamline 9.1 - Spinning Capillary run on Developmental Image Plate System (minimal FWHM ~ 0.05° 2-theta) 
  • Filename: aldsync.* 
  • Run on Graham Bushnell-Wye, et al. 
  • Beam width and height: 0.5mmx0.5mm X-ray beam 
  • Wavelength: 0.692 A 
  • Distance from Sample to curved image plate: 350 mm 
  • Start, Step, Stop: 2.115, 0.005, 40.000 
  • Counting time: 5 hours 
  • Sample Holder: Sample packed in 0.5mm glass capilliary, 
  • References: 
    • "Development of Curved Image-Plate Techniques for Studies of Powder Diffraction, Liquids and Amorphous Materials",

    • M.A. Roberts, J. L. Finney, G. Bushnell-Wye 
      Proceedings of EPDIC-5, Parma, Italy, 1997. 
    • "Developments and Time-Resolved Studies using a Curved Image-Plate Detector",

    • M.A. Roberts, J. L. Finney, G. Bushnell-Wye, W. A. Steer, Manuscript in Preparation. 



Copyright © 1998 L.M.D Cranswick & A. Le Bail


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Please feel free to email any queries to Lachlan Cranswick at: [email protected]