EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005slh0412

Report generated Aug 15, 2005; 10:59:42

Unit cell

5232 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)10.5324 +/- 0.0002
b (Angstrom)14.7346 +/- 0.0003
c (Angstrom)15.2645 +/- 0.0004
alpha (°) 90.000
beta (°)94.9878 +/- 0.0011
gamma (°) 90.000
Volume (A**3)2359.94 +/- 0.09
Mosaicity (°)0.5270 +/- 0.0010

Data collection


Total number of images collected145
Total exposure time47.5 minutes
Data collection exposure time46.2 minutes
Data collection wall-clock time57.0 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.70 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f137274.0° phi2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 122
Overload or incomplete profile 902
Sigma cutoff  41
High resolution limit   6

Final Data Set

Scale factor range7.77-10.00
Number of 'full' reflections 14539
Number of 'partial' reflections  8641
Total number of integrated reflections 21575
Total number of unique reflections  5585
Data completeness  99.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  222.7
Average Sigma(I)    5.9
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 19215 reflections reduced R(int) from 0.0873 to 0.0319

Before rejection, 22466 reflections total and 5611 unique

After rejection, 22133 reflections total and 5609 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.1  0.0321   0.784 - 1.087   0.815 - 1.321   1.501   22133   19448
Ratio of minimum to maximum apparent transmission: 0.616980


  Group    Personal  
  Operator   Mike Hursthouse  
  Sample Owner   SLH  
  Local Code   SLH0412  
  Formula   C31H38N2O4P2S4Hg1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.4 x 0.35 x 0.2 (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    'graphite'
_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/