EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2007jmw001

Report generated Jan 30, 2007; 13:23:56

Unit cell

3681 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)4.95090 +/- 0.00010
b (Angstrom)7.8949 +/- 0.0003
c (Angstrom)18.7419 +/- 0.0007
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)732.56 +/- 0.04
Mosaicity (°)0.349 +/- 0.002

Data collection


Total number of images collected147
Total exposure time118.3 minutes
Data collection exposure time116.3 minutes
Data collection wall-clock time128.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f84168.0° phi2.000°50 secondsYes
data collections02f55110.0° omega2.000°50 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected  39
Overload or incomplete profile 162
Sigma cutoff   6
High resolution limit  11

Final Data Set

Scale factor range10.00-10.65
Number of 'full' reflections  5613
Number of 'partial' reflections  1968
Total number of integrated reflections  7338
Total number of unique reflections  1035
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  101.6
Average Sigma(I)    2.5
Overall R-merge (linear)  0.047

Sadabs Results

Parameter refinement on 6343 reflections reduced R(int) from 0.0651 to 0.0419

Before rejection, 7302 reflections total and 1041 unique

After rejection, 7228 reflections total and 1041 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0441   0.867 - 0.956   0.952 - 1.150   1.247    4340    3895
    2    6.5  0.0441   0.932 - 1.009   0.921 - 1.135   1.242    2888    2577
Ratio of minimum to maximum apparent transmission: 0.801073


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CC47809  
  Formula   C7 H8 O3 S  
  Crystal Colour   Clear Colourless  
  Crystal Habit   Cut Needle  
  Crystal Size   0.42 x 0.06 x 0.04 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

      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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

'COLLECT (Hooft, R.W.W., 1998)'
'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
'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. (2003). SADABS. Version 2.10. 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/