EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005slh0404

Report generated Apr 04, 2005; 13:09:25

Unit cell

7468 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)12.10340 +/- 0.00010
b (Angstrom)17.5079 +/- 0.0002
c (Angstrom)15.3300 +/- 0.0002
alpha (°) 90.000
beta (°)99.0344 +/- 0.0008
gamma (°) 90.000
Volume (A**3)3208.21 +/- 0.06
Mosaicity (°)0.3890 +/- 0.0010

Data collection


Total number of images collected345
Total exposure time75.0 minutes
Data collection exposure time74.2 minutes
Data collection wall-clock time102.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f227227.0° phi1.000°13 secondsYes
data collections02f110110.0° omega1.000°13 secondsYes
Phi/Chii01f - i08f86 seconds

Scalepack Scaling

Deleted observations

Rejected 171
Zero sigma or profile test   7
Overload or incomplete profile 988
Sigma cutoff  18

Final Data Set

Scale factor range8.46-10.13
Number of 'full' reflections 18883
Number of 'partial' reflections 20982
Total number of integrated reflections 37963
Total number of unique reflections  7592
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   55.0
Average Sigma(I)    1.9
Overall R-merge (linear)  0.039

Sadabs Results

Parameter refinement on 30028 reflections reduced R(int) from 0.0535 to 0.0337

Before rejection, 39005 reflections total and 7595 unique

After rejection, 38707 reflections total and 7593 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0371   0.910 - 1.008   0.921 - 1.185   1.154   26191   21293
    2   -6.8  0.0372   0.856 - 1.038   0.933 - 1.161   1.204   12516   10101
Ratio of minimum to maximum apparent transmission: 0.776887


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 144a  
  Formula   C28 H32 N2 O4 P2 S4 Cd1  
  Crystal Colour    Colourless  
  Crystal Habit    Prism  
  Crystal Size   0.28 x 0.24 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 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/