EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04sjc0831

Report generated Oct 05, 2004; 15:31:52

Unit cell

3533 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)8.3298 +/- 0.0004
b (Angstrom)16.5088 +/- 0.0005
c (Angstrom)20.1072 +/- 0.0009
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)2765.0 +/- 0.2
Mosaicity (°)0.767 +/- 0.002

Data collection


Total number of images collected232
Total exposure time39.5 minutes
Data collection exposure time38.1 minutes
Data collection wall-clock time56.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f183183.0° phi1.000°10 secondsYes
data collections02f41 41.0° omega1.000°10 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 151
Zero sigma or profile test   9
Overload or incomplete profile 838
Sigma cutoff  17
High resolution limit   9

Final Data Set

Scale factor range7.48-10.89
Number of 'full' reflections  2412
Number of 'partial' reflections 20691
Total number of integrated reflections 22172
Total number of unique reflections  3591
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   24.7
Average Sigma(I)    1.5
Overall R-merge (linear)  0.098

Sadabs Results

Parameter refinement on 10388 reflections reduced R(int) from 0.1237 to 0.0578

Before rejection, 22005 reflections total and 3595 unique

After rejection, 21771 reflections total and 3595 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0905   0.766 - 1.247   0.913 - 1.444   1.275   17784    9470
    2   -2.5  0.1152   0.498 - 0.555   0.922 - 1.328   1.306    3987    1917
Ratio of minimum to maximum apparent transmission: 0.631892


  Group    Personal  
  Operator   Simon Coles  
  Sample Owner   Esther Rousay  
  Local Code   OHBOCP  
  Formula   C14H20O5  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size  0.25 x 0.17 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/