EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/2007src1050

Report generated Aug 06, 2007; 13:07:32

Unit cell

20793 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)7.7257 +/- 0.0002
b (Angstrom)21.1223 +/- 0.0007
c (Angstrom)11.5315 +/- 0.0002
alpha (°) 90.000
beta (°)96.6536 +/- 0.0017
gamma (°) 90.000
Volume (A**3)1869.09 +/- 0.09
Mosaicity (°)0.5380 +/- 0.0010

Data collection

Summary

Total number of images collected292
Total exposure time116.5 minutes
Data collection exposure time115.1 minutes
Data collection wall-clock time131.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f222355.2° phi1.600°24 secondsYes
data collections02f31 49.6° omega1.600°24 secondsYes
data collections03f31 49.6° omega1.600°24 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Overload or incomplete profile 812
Sigma cutoff 381
High resolution limit  27

Final Data Set

Scale factor10.00
Number of 'full' reflections 13408
Number of 'partial' reflections 11969
Total number of integrated reflections 23524
Total number of unique reflections  4372
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   87.7
Average Sigma(I)    2.4
Overall R-merge (linear)  0.203

Sadabs Results

Parameter refinement on 17847 reflections reduced R(int) from 0.1638 to 0.0546

Before rejection, 24269 reflections total and 4391 unique

After rejection, 21359 reflections total and 4381 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.0639   0.674 - 1.283   0.952 - 1.114   2.043   16821   11995
    2   12.0  0.0415   0.633 - 0.741   0.934 - 1.070   1.953    2273    1721
    3   12.0  0.0450   0.663 - 0.746   0.939 - 1.097   1.978    2265    1683
Ratio of minimum to maximum apparent transmission: 0.838105

Metadata

  Group    Service  
  Operator   Richard Stephenson  
  Sample Owner   Dr Adrian Dobbs  
  Local Code   ex 303.4Cr228+  
  Formula   C20H30ClNO2S  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.26 x 0.06 x 0.02 (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/