EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005slh0408

Report generated Jul 27, 2005; 08:34:10

Unit cell

5532 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)10.5379 +/- 0.0003
b (Angstrom)14.7376 +/- 0.0002
c (Angstrom)15.2670 +/- 0.0003
alpha (°) 90.000
beta (°)95.0039 +/- 0.0009
gamma (°) 90.000
Volume (A**3)2361.98 +/- 0.09
Mosaicity (°)0.5790 +/- 0.0010

Data collection


Total number of images collected177
Total exposure time30.1 minutes
Data collection exposure time28.8 minutes
Data collection wall-clock time43.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.80 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f136272.0° phi2.000°10 secondsYes
data collections02f33 66.0° omega2.000°10 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 162
Overload or incomplete profile1170
Sigma cutoff  20
High resolution limit  11

Final Data Set

Scale factor range8.13-11.31
Number of 'full' reflections 16731
Number of 'partial' reflections 11621
Total number of integrated reflections 27197
Total number of unique reflections  5626
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  456.0
Average Sigma(I)    9.4
Overall R-merge (linear)  0.042

Sadabs Results

Parameter refinement on 24011 reflections reduced R(int) from 0.0893 to 0.0341

Before rejection, 27060 reflections total and 5640 unique

After rejection, 26739 reflections total and 5637 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.2  0.0329   0.898 - 1.130   0.853 - 1.504   1.515   21518   19393
    2   -7.6  0.0425   0.588 - 0.861   0.895 - 1.636   1.578    5221    4634
Ratio of minimum to maximum apparent transmission: 0.521653


  Group    Personal  
  Operator   Mike Hursthouse  
  Sample Owner   S L Huth  
  Local Code   137a  
  Formula   C18H24O4P2S4Hg1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.25 x 0.15 x 0.09 (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/