EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2007src0763/2007src0763

Report generated Jun 28, 2007; 17:10:33

Unit cell

12908 reflections with 2.91°<theta<28.70° (resolution between 7.00A and 0.74A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)9.3800 +/- 0.0003
b (Angstrom)12.9924 +/- 0.0004
c (Angstrom)15.4076 +/- 0.0003
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1877.70 +/- 0.09
Mosaicity (°)0.531 +/- 0.002

Data collection


Total number of images collected156
Total exposure time35.5 minutes
Data collection exposure time34.1 minutes
Data collection wall-clock time40.1 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f115172.5° phi1.500°13 secondsYes
data collections02f33 49.5° omega1.500°13 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Overload or incomplete profile 474
Sigma cutoff  50
High resolution limit   3

Final Data Set

Scale factor10.00
Number of 'full' reflections  6807
Number of 'partial' reflections  6578
Total number of integrated reflections 12808
Total number of unique reflections  2751
Data completeness  99.5%
Resolution range7.00-0.74 A
Theta range2.91°-28.70°
Average Intensity  140.1
Average Sigma(I)    3.2
Overall R-merge (linear)  0.088

Sadabs Results

Estimated minimum and maximum transmission: 0.6519 0.7458


  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr F. H. Fry  
  Local Code   wxp 249 Gr38+  
  Formula   C19 H28 Cl1 N1 O2 S1  
  Crystal Colour    Colourless  
  Crystal Habit    Rod  
  Crystal Size   0.24 x 0.1 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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

'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. (2007). SADABS. Version 2007/2. 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/