EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0078

Report generated Feb 07, 2007; 13:35:53

Unit cell

1775 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)7.8090 +/- 0.0004
b (Angstrom)7.3341 +/- 0.0002
c (Angstrom)13.4109 +/- 0.0007
alpha (°) 90.000
beta (°)104.986 +/- 0.002
gamma (°) 90.000
Volume (A**3)741.94 +/- 0.06
Mosaicity (°)0.503 +/- 0.003

Data collection


Total number of images collected188
Total exposure time62.3 minutes
Data collection exposure time61.0 minutes
Data collection wall-clock time248.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f133266.0° phi2.000°20 secondsYes
data collections02f47 94.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 216
Zero sigma or profile test   3
Overload or incomplete profile 288
Sigma cutoff  69
High resolution limit  56

Final Data Set

Scale factor range7.97-11.82
Number of 'full' reflections  5219
Number of 'partial' reflections  2950
Total number of integrated reflections  7799
Total number of unique reflections  1816
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   50.8
Average Sigma(I)    1.4
Overall R-merge (linear)  0.065

Sadabs Results

Parameter refinement on 6094 reflections reduced R(int) from 0.1164 to 0.0552

Before rejection, 8041 reflections total and 1851 unique

After rejection, 7138 reflections total and 1842 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0527   0.708 - 0.919   0.933 - 1.067   1.990    5298    4070
    2   11.1  0.0639   0.708 - 1.207   0.973 - 1.090   2.075    1840    1344
Ratio of minimum to maximum apparent transmission: 0.855958


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. E. McDonald  
  Local Code   LAS-1037-241 (n)  
  Formula   C7 H8 N4 O2  
  Crystal Colour    Colourless  
  Crystal Habit    Needle  
  Crystal Size   0.52 x 0.08 x 0.03 (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/