EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2008src0176

Report generated Feb 25, 2008; 11:29:51

Unit cell

6613 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)3.92460 +/- 0.00010
b (Angstrom)16.0687 +/- 0.0005
c (Angstrom)17.4699 +/- 0.0004
alpha (°) 90.000
beta (°)90.8247 +/- 0.0017
gamma (°) 90.000
Volume (A**3)1101.59 +/- 0.05
Mosaicity (°)0.336 +/- 0.002

Data collection

Summary

Total number of images collected196
Total exposure time104.3 minutes
Data collection exposure time101.0 minutes
Data collection wall-clock time120.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f93186.0° phi2.000°32 secondsYes
data collections02f17 34.0° omega2.000°32 secondsYes
data collections03f23 46.0° omega2.000°32 secondsYes
data collections04f55110.0° omega2.000°32 secondsYes
Phi/Chii01f - i08f825 seconds

Scalepack Scaling

Deleted observations

Rejected  10
Overload or incomplete profile 270
Sigma cutoff  19
High resolution limit  15

Final Data Set

Scale factor10.00
Number of 'full' reflections 11525
Number of 'partial' reflections  3953
Total number of integrated reflections 15050
Total number of unique reflections  2600
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   61.2
Average Sigma(I)    2.0
Overall R-merge (linear)  0.062

Sadabs Results

Estimated minimum and maximum transmission: 0.6637 0.7456

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Prof PJ Skabara  
  Local Code   TW TTF  
  Formula   C26H12S8  
  Crystal Colour    Yellow  
  Crystal Habit    Block  
  Crystal Size   0.12 x 0.04 x 0.02 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using  SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate  (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file


Southampton CIF entry fields

_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '9.091'

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. (2007). SADABS. Version 2007/2. Bruker AXS Inc., Madison, Wisconsin, USA.

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/