EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0019

Report generated Feb 18, 2007; 11:13:06

Unit cell

3719 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)11.8889 +/- 0.0005
b (Angstrom)6.2180 +/- 0.0003
c (Angstrom)21.9456 +/- 0.0009
alpha (°) 90.000
beta (°)104.848 +/- 0.002
gamma (°) 90.000
Volume (A**3)1568.16 +/- 0.12
Mosaicity (°)0.682 +/- 0.002

Data collection


Total number of images collected251
Total exposure time133.6 minutes
Data collection exposure time130.9 minutes
Data collection wall-clock time140.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f180288.0° phi1.600°32 secondsYes
data collections02f63100.8° omega1.600°32 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 394
Zero sigma or profile test   4
Overload or incomplete profile 494
Sigma cutoff 258
High resolution limit  21

Final Data Set

Scale factor range9.42-13.77
Number of 'full' reflections  6904
Number of 'partial' reflections  9067
Total number of integrated reflections 14785
Total number of unique reflections  3899
Data completeness  99.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   26.4
Average Sigma(I)    1.1
Overall R-merge (linear)  0.083

Sadabs Results

Parameter refinement on 10170 reflections reduced R(int) from 0.1344 to 0.0538

Before rejection, 15749 reflections total and 3936 unique

After rejection, 13653 reflections total and 3899 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0622   0.763 - 1.415   0.987 - 1.138   2.068   10109    6471
    2   14.6  0.0579   0.511 - 0.876   0.990 - 1.165   2.038    3544    2247
Ratio of minimum to maximum apparent transmission: 0.847342


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp8 e5  
  Formula   C12H27O4N1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.12 x 0.1 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    '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/