EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0003

Report generated Jan 28, 2006; 20:11:39

Unit cell

1084 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)6.0084 +/- 0.0008
b (Angstrom)9.6903 +/- 0.0013
c (Angstrom)8.1526 +/- 0.0013
alpha (°) 90.000
beta (°)90.039 +/- 0.008
gamma (°) 90.000
Volume (A**3)474.67 +/- 0.12
Mosaicity (°)1.965 +/- 0.008

Data collection


Total number of images collected193
Total exposure time189.7 minutes
Data collection exposure time185.6 minutes
Data collection wall-clock time199.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance33.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f128256.0° phi2.000°60 secondsYes
data collections02f57114.0° omega2.000°60 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected  72
Zero sigma or profile test   1
Overload or incomplete profile 366
Sigma cutoff  15
High resolution limit  55

Final Data Set

Scale factor range10.00-17.38
Number of 'full' reflections    11
Number of 'partial' reflections  5561
Total number of integrated reflections  4996
Total number of unique reflections  1149
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   59.3
Average Sigma(I)    3.0
Overall R-merge (linear)  0.084

Sadabs Results

Parameter refinement on 3507 reflections reduced R(int) from 0.1746 to 0.0577

Before rejection, 5451 reflections total and 1163 unique

After rejection, 5340 reflections total and 1163 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   10.1  0.0810   0.782 - 1.003   0.880 - 1.611   1.411    3673    2388
    2   -9.6  0.0583   0.709 - 1.054   0.879 - 1.418   1.242    1667    1315
Ratio of minimum to maximum apparent transmission: 0.545641


  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp5 b2  
  Formula   C4H6N2  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.1 x 0.04 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/