EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2009src0062

Report generated Jan 21, 2009; 17:49:52

Unit cell

8933 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)12.6554 +/- 0.0005
b (Angstrom)8.2142 +/- 0.0004
c (Angstrom)13.5783 +/- 0.0007
alpha (°) 90.000
beta (°)103.052 +/- 0.003
gamma (°) 90.000
Volume (A**3)1375.06 +/- 0.11
Mosaicity (°)0.522 +/- 0.003

Data collection


Total number of images collected195
Total exposure time158.8 minutes
Data collection exposure time156.8 minutes
Data collection wall-clock time164.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f136272.0° phi2.000°50 secondsYes
data collections02f51102.0° omega2.000°50 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Overload or incomplete profile 354
Sigma cutoff 443
High resolution limit 118

Final Data Set

Scale factor10.00
Number of 'full' reflections 10068
Number of 'partial' reflections  5950
Total number of integrated reflections 15009
Total number of unique reflections  3348
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   30.0
Average Sigma(I)    1.8
Overall R-merge (linear)  0.287

Sadabs Results

Estimated minimum and maximum transmission: 0.6039 0.7456


  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   HP139  
  Formula   C14H17N5O  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.15 x 0.04 x 0.01 (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    '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

'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/