EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0079

Report generated Dec 06, 2006; 11:27:58

Unit cell

1566 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)5.7939 +/- 0.0002
b (Angstrom)7.4320 +/- 0.0005
c (Angstrom)15.9222 +/- 0.0010
alpha (°) 90.000
beta (°)96.290 +/- 0.004
gamma (°) 90.000
Volume (A**3)681.49 +/- 0.07
Mosaicity (°)0.673 +/- 0.003

Data collection


Total number of images collected188
Total exposure time124.7 minutes
Data collection exposure time120.6 minutes
Data collection wall-clock time134.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f163326.0° phi2.000°40 secondsYes
data collections02f17 34.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected  64
Zero sigma or profile test   2
Overload or incomplete profile 198
Sigma cutoff  19
High resolution limit  47

Final Data Set

Scale factor range9.74-10.36
Number of 'full' reflections  4937
Number of 'partial' reflections  4083
Total number of integrated reflections  8650
Total number of unique reflections  1678
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   68.6
Average Sigma(I)    2.4
Overall R-merge (linear)  0.051

Sadabs Results

Parameter refinement on 6125 reflections reduced R(int) from 0.0616 to 0.0441

Before rejection, 8763 reflections total and 1696 unique

After rejection, 8603 reflections total and 1694 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0514   0.909 - 1.050   0.939 - 1.162   1.281    7854    5909
    2   -7.1  0.0455   0.549 - 0.614   0.936 - 1.138   1.201     749     523
Ratio of minimum to maximum apparent transmission: 0.805736


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp15 c1  
  Formula   C11H17O3N2S1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.2 x 0.06 x 0.03 (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/