EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0072

Report generated Nov 22, 2006; 13:14:16

Unit cell

3064 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)11.6392 +/- 0.0017
b (Angstrom)6.2916 +/- 0.0008
c (Angstrom)22.244 +/- 0.003
alpha (°) 90.000
beta (°)96.166 +/- 0.007
gamma (°) 90.000
Volume (A**3)1619.5 +/- 0.4
Mosaicity (°)1.321 +/- 0.006

Data collection


Total number of images collected205
Total exposure time203.1 minutes
Data collection exposure time197.7 minutes
Data collection wall-clock time258.0 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f124186.0° phi1.500°60 secondsYes
data collections02f73109.5° omega1.500°60 secondsYes
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Rejected 119
Zero sigma or profile test 198
Overload or incomplete profile 692
Sigma cutoff 228

Final Data Set

Scale factor range7.19-10.64
Number of 'full' reflections   624
Number of 'partial' reflections 15063
Total number of integrated reflections 11530
Total number of unique reflections  3678
Data completeness  88.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity    8.4
Average Sigma(I)    1.9
Overall R-merge (linear)  0.180

Sadabs Results

Parameter refinement on 4522 reflections reduced R(int) from 0.1375 to 0.0847

Before rejection, 15194 reflections total and 3994 unique

After rejection, 14684 reflections total and 3984 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.2270   0.725 - 0.963   0.826 - 1.564   1.224    9454    3843
    2   -6.8  0.3047   0.785 - 1.009   0.864 - 2.115   1.288    5230    1657
Ratio of minimum to maximum apparent transmission: 0.390584


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp15 c4  
  Formula   C14H26O3N1S1  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.23 x 0.11 x 0.02 (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/