EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/05src0190

Report generated Feb 11, 2005; 13:01:43

Unit cell

4407 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)8.4369 +/- 0.0002
b (Angstrom)16.8514 +/- 0.0004
c (Angstrom)24.3974 +/- 0.0006
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)3468.67 +/- 0.14
Mosaicity (°)0.4730 +/- 0.0010

Data collection


Total number of images collected438
Total exposure time110.4 minutes
Data collection exposure time109.0 minutes
Data collection wall-clock time143.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance45.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f157157.0° phi1.000°15 secondsYes
data collections02f138138.0° omega1.000°15 secondsYes
data collections03f135135.0° omega1.000°15 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test  15
Overload or incomplete profile1366
Sigma cutoff  15
High resolution limit 186

Final Data Set

Scale factor range9.94-16.44
Number of 'full' reflections 10090
Number of 'partial' reflections 15177
Total number of integrated reflections 23474
Total number of unique reflections  4424
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   46.7
Average Sigma(I)    1.7
Overall R-merge (linear)  0.075

Sadabs Results

Parameter refinement on 24217 reflections reduced R(int) from 0.4881 to 0.0679

Before rejection, 32334 reflections total and 4488 unique

After rejection, 18943 reflections total and 3689 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0774   0.699 - 0.987   0.939 - 1.174   1.607    7097    5192
    2  -18.3  0.0738   0.741 - 0.977   0.969 - 1.280   1.667    5874    4213
    3  -18.3  0.0631   0.927 - 1.486   0.941 - 1.210   1.692    5972    4475
Ratio of minimum to maximum apparent transmission: 0.733113


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. P. J. Skabara  
  Local Code   HSunsub  
  Formula   C20 H20 O4 S1  
  Crystal Colour   Pale Yellow  
  Crystal Habit    Rod  
  Crystal Size   0.24 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    '10cm confocal mirrors'
_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/