EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/07skc0007

Report generated Feb 09, 2007; 10:20:51

Unit cell

1536 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)6.313 +/- 0.005
b (Angstrom)11.581 +/- 0.010
c (Angstrom)16.678 +/- 0.013
alpha (°)78.42 +/- 0.05
beta (°)89.90 +/- 0.06
gamma (°)89.94 +/- 0.05
Volume (A**3)1194.6 +/- 1.7
Mosaicity (°)5.60 +/- 0.02

Data collection


Total number of images collected203
Total exposure time7.2 hours
Data collection exposure time7.1 hours
Data collection wall-clock time8.8 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance33.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f181362.0° phi2.000°130 secondsYes
data collections02f13 26.0° omega2.000°130 secondsYes
Phi/Chii01f - i08f850 seconds

Scalepack Scaling

Deleted observations

Rejected 104
Zero sigma or profile test 171
Overload or incomplete profile 832
Sigma cutoff1248
High resolution limit1418

Final Data Set

Scale factor range6.67-10.72
Number of 'full' reflections     0
Number of 'partial' reflections  9943
Total number of integrated reflections  5263
Total number of unique reflections  2920
Data completeness  55.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   27.4
Average Sigma(I)    4.6
Overall R-merge (linear)  0.115

Sadabs Results

Parameter refinement on 3125 reflections reduced R(int) from 0.1302 to 0.0654

Before rejection, 10679 reflections total and 4750 unique

After rejection, 9085 reflections total and 4538 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   13.5  0.1606   0.727 - 0.965   0.744 - 9.900   2.259    8757    2640
    2   12.9  0.2261   0.665 - 0.854   0.765 - 5.455   2.199     328      93
Ratio of minimum to maximum apparent transmission: 0.075114


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp14 a4  
  Formula   C12H23O4N1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.17 x 0.1 x 0.01 (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/