EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0048

Report generated Sep 07, 2006; 19:58:40

Unit cell

1195 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)4.6392 +/- 0.0009
b (Angstrom)10.4056 +/- 0.0016
c (Angstrom)22.888 +/- 0.004
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1104.9 +/- 0.3
Mosaicity (°)1.601 +/- 0.008

Data collection


Total number of images collected175
Total exposure time61.1 minutes
Data collection exposure time59.1 minutes
Data collection wall-clock time78.0 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f167233.8° phi1.400°21 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected  88
Zero sigma or profile test  58
Overload or incomplete profile 448
Sigma cutoff  23
High resolution limit  51

Final Data Set

Scale factor range9.85-11.23
Number of 'full' reflections     0
Number of 'partial' reflections  6928
Total number of integrated reflections  5302
Total number of unique reflections  1377
Data completeness  91.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   12.8
Average Sigma(I)    1.5
Overall R-merge (linear)  0.152

Sadabs Results

Parameter refinement on 3231 reflections reduced R(int) from 0.2011 to 0.0831

Before rejection, 7354 reflections total and 1476 unique

After rejection, 7004 reflections total and 1474 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.1554   0.622 - 0.927   0.706 - 5.719   1.350    7004    3371
Ratio of minimum to maximum apparent transmission: 0.123373


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 e4  
  Formula   C10H16O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.12 x 0.1 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/