EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2008lsh117

Report generated Nov 07, 2008; 11:39:57

Unit cell

30114 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)3.8114 +/- 0.0004
b (Angstrom)11.3360 +/- 0.0014
c (Angstrom)18.3264 +/- 0.0017
alpha (°) 90.000
beta (°) 90.058
gamma (°) 90.000
Volume (A**3)791.81 +/- 0.15
Mosaicity (°)2.792 +/- 0.006

Data collection


Total number of images collected213
Total exposure time14.3 hours
Data collection exposure time14.1 hours
Data collection wall-clock time15.6 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f101191.9° phi1.900°247 secondsYes
data collections02f54102.6° omega1.900°247 secondsYes
data collections03f50 95.0° omega1.900°247 secondsYes
Phi/Chii01f - i08f880 seconds

Scalepack Scaling

Deleted observations

Rejected  23
Overload or incomplete profile 560
Sigma cutoff  21

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 10073
Total number of integrated reflections  8316
Total number of unique reflections  1880
Data completeness  99.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  208.5
Average Sigma(I)    7.4
Overall R-merge (linear)  0.082

Sadabs Results

Estimated minimum and maximum transmission: 0.5316 0.7456


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   OAA/CN  
  Formula   C9 H8 N2 O1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Needle  
  Crystal Size   0.16 x 0.1 x 0.08 (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/