EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0051

Report generated Sep 10, 2006; 18:55:41

Unit cell

2165 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)3.9015 +/- 0.0002
b (Angstrom)17.3293 +/- 0.0010
c (Angstrom)13.8628 +/- 0.0007
alpha (°) 90.000
beta (°)96.299 +/- 0.003
gamma (°) 90.000
Volume (A**3)931.61 +/- 0.09
Mosaicity (°)0.666 +/- 0.003

Data collection


Total number of images collected170
Total exposure time89.0 minutes
Data collection exposure time87.0 minutes
Data collection wall-clock time100.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f113226.0° phi2.000°32 secondsYes
data collections02f49 98.0° omega2.000°32 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected 142
Overload or incomplete profile 326
Sigma cutoff   3
High resolution limit  27

Final Data Set

Scale factor range7.20-17.13
Number of 'full' reflections  5605
Number of 'partial' reflections  5052
Total number of integrated reflections 10289
Total number of unique reflections  2200
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   38.2
Average Sigma(I)    1.7
Overall R-merge (linear)  0.090

Sadabs Results

Parameter refinement on 6459 reflections reduced R(int) from 0.1829 to 0.0611

Before rejection, 10249 reflections total and 2211 unique

After rejection, 10034 reflections total and 2210 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0760   1.163 - 2.003   0.808 - 1.188   1.402    6954    4506
    2   -7.8  0.0641   0.275 - 0.497   0.815 - 1.162   1.289    3080    2243
Ratio of minimum to maximum apparent transmission: 0.680391


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 d3  
  Formula   C8H12O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.1 x 0.07 x 0.06 (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/