EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005slh0403

Report generated Apr 04, 2005; 12:14:51

Unit cell

7335 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)11.9818 +/- 0.0002
b (Angstrom)17.7085 +/- 0.0003
c (Angstrom)15.2362 +/- 0.0002
alpha (°) 90.000
beta (°)101.7881 +/- 0.0009
gamma (°) 90.000
Volume (A**3)3164.63 +/- 0.09
Mosaicity (°)0.6760 +/- 0.0010

Data collection


Total number of images collected405
Total exposure time35.2 minutes
Data collection exposure time34.5 minutes
Data collection wall-clock time69.1 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f287287.0° phi1.000°5 secondsYes
data collections02f110110.0° omega1.000°5 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 223
Zero sigma or profile test   6
Overload or incomplete profile1650
Sigma cutoff  20
High resolution limit  33

Final Data Set

Scale factor range9.17-10.18
Number of 'full' reflections  8093
Number of 'partial' reflections 37773
Total number of integrated reflections 42407
Total number of unique reflections  7486
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   54.7
Average Sigma(I)    1.9
Overall R-merge (linear)  0.042

Sadabs Results

Parameter refinement on 33293 reflections reduced R(int) from 0.0631 to 0.0347

Before rejection, 45200 reflections total and 7500 unique

After rejection, 44788 reflections total and 7499 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0401   0.903 - 1.029   0.944 - 1.239   1.208   32514   25163
    2   -6.8  0.0395   0.857 - 0.987   0.943 - 1.235   1.232   12274    9437
Ratio of minimum to maximum apparent transmission: 0.760864


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 145  
  Formula   C28 H30 N2 O4 P2 S4 Cd1  
  Crystal Colour    Colourless  
  Crystal Habit    Prism  
  Crystal Size   0.38 x 0.36 x 0.1 (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/