EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/2007src1375

Report generated Oct 19, 2007; 17:13:10

Unit cell

9689 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p222
a (Angstrom)5.6923 +/- 0.0003
b (Angstrom)8.3358 +/- 0.0006
c (Angstrom)26.3096 +/- 0.0017
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1248.39 +/- 0.14
Mosaicity (°)0.857 +/- 0.003

Data collection

Summary

Total number of images collected238
Total exposure time194.2 minutes
Data collection exposure time192.9 minutes
Data collection wall-clock time211.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance42.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f77154.0° phi2.000°50 secondsYes
data collections02f33 66.0° omega2.000°50 secondsYes
data collections03f59118.0° omega2.000°50 secondsYes
data collections04f61122.0° omega2.000°50 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test   1
Overload or incomplete profile 476
Sigma cutoff 231
High resolution limit  96

Final Data Set

Scale factor10.00
Number of 'full' reflections  4941
Number of 'partial' reflections  6106
Total number of integrated reflections  9250
Total number of unique reflections  1689
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  189.8
Average Sigma(I)    4.2
Overall R-merge (linear)  0.262

Sadabs Results

Parameter refinement on 7558 reflections reduced R(int) from 0.3017 to 0.0787

Before rejection, 10404 reflections total and 1719 unique

After rejection, 8764 reflections total and 1712 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   20.2  0.0706   0.439 - 1.225   0.935 - 1.562   2.154    2899    1978
    2   19.6  0.0588   0.811 - 0.969   0.935 - 1.126   1.955    1076     800
    3   15.6  0.0719   0.491 - 0.859   0.934 - 1.296   2.116    2234    1591
    4   19.6  0.0560   0.618 - 1.058   0.934 - 1.292   1.991    2555    1819
Ratio of minimum to maximum apparent transmission: 0.597665

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Skabara  
  Local Code   IA Fused  
  Formula   C22H12S3  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.26 x 0.15 x 0.005 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      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'

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'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
_computing_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/