EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2007may0004

Report generated Jun 08, 2007; 09:39:03

Unit cell

6958 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)22.2439 +/- 0.0016
b (Angstrom)5.1189 +/- 0.0002
c (Angstrom)15.6071 +/- 0.0010
alpha (°) 90.000
beta (°)95.838 +/- 0.003
gamma (°) 90.000
Volume (A**3)1767.87 +/- 0.18
Mosaicity (°)0.557 +/- 0.003

Data collection


Total number of images collected229
Total exposure time6.8 hours
Data collection exposure time6.8 hours
Data collection wall-clock time7.0 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f96192.0° phi2.000°110 secondsYes
data collections02f16 32.0° omega2.000°110 secondsYes
data collections03f52104.0° omega2.000°110 secondsYes
data collections04f57114.0° omega2.000°110 secondsYes
Phi/Chii01f - i08f835 seconds

Scalepack Scaling

Deleted observations

Rejected  60
Zero sigma or profile test   2
Overload or incomplete profile 196
Sigma cutoff  43
High resolution limit  19

Final Data Set

Scale factor range9.43-10.24
Number of 'full' reflections  7332
Number of 'partial' reflections  4556
Total number of integrated reflections 11536
Total number of unique reflections  2259
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   30.5
Average Sigma(I)    1.8
Overall R-merge (linear)  0.083

Sadabs Results

Estimated minimum and maximum transmission: 0.6213 0.7456


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CC46101  
  Formula   C11 H8 O3  
  Crystal Colour    Colourless  
  Crystal Habit   Split Plate  
  Crystal Size   0.3 x 0.06 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 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/