EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2008skc0001

Report generated Oct 09, 2008; 13:29:46

Unit cell

5405 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)6.9977 +/- 0.0003
b (Angstrom)8.3790 +/- 0.0003
c (Angstrom)9.2501 +/- 0.0003
alpha (°)116.302 +/- 0.002
beta (°)101.825 +/- 0.002
gamma (°)91.149 +/- 0.002
Volume (A**3)472.08 +/- 0.03
Mosaicity (°)0.372 +/- 0.002

Data collection


Total number of images collected335
Total exposure time100.7 minutes
Data collection exposure time99.3 minutes
Data collection wall-clock time125.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f171342.0° phi2.000°18 secondsYes
data collections02f23 46.0° omega2.000°18 secondsYes
data collections03f23 46.0° omega2.000°18 secondsYes
data collections04f55110.0° omega2.000°18 secondsYes
data collections05f55110.0° omega2.000°18 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   8
Zero sigma or profile test   2
Overload or incomplete profile 216
Sigma cutoff  29
High resolution limit  65

Final Data Set

Scale factor10.00
Number of 'full' reflections  8283
Number of 'partial' reflections  3166
Total number of integrated reflections 11104
Total number of unique reflections  2143
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   62.0
Average Sigma(I)    2.0
Overall R-merge (linear)  0.069

Sadabs Results

Estimated minimum and maximum transmission: 0.6556 0.7456


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   MnA Im  
  Formula   C6H8O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.19 x 0.09 x 0.07 (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 2007/2 (Sheldrick, G.M., 2007)'

_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 Roper 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. (2007). SADABS. Version 2007/2. 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/