EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2009src0671

Report generated Jul 10, 2009; 14:32:50

Unit cell

9591 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
c2
a (Angstrom)18.9488 +/- 0.0006
b (Angstrom)5.60240 +/- 0.00010
c (Angstrom)20.7934 +/- 0.0006
alpha (°) 90.000
beta (°)90.3551 +/- 0.0016
gamma (°) 90.000
Volume (A**3)2207.36 +/- 0.10
Mosaicity (°)0.450 +/- 0.002

Data collection

Summary

Total number of images collected258
Total exposure time136.0 minutes
Data collection exposure time134.7 minutes
Data collection wall-clock time150.6 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance33.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f123196.8° phi1.600°32 secondsYes
data collections02f67107.2° omega1.600°32 secondsYes
data collections03f60 96.0° omega1.600°32 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test   3
Overload or incomplete profile 314
Sigma cutoff  91
Low resolution limit   8

Final Data Set

Scale factor10.00
Number of 'full' reflections  7821
Number of 'partial' reflections  5062
Total number of integrated reflections 12385
Total number of unique reflections  2791
Data completeness  99.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   53.1
Average Sigma(I)    1.8
Overall R-merge (linear)  0.144

Sadabs Results

Parameter refinement on 10284 reflections reduced R(int) from 0.0982 to 0.0604

Before rejection, 12322 reflections total and 2794 unique

After rejection, 10903 reflections total and 2776 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   13.5  0.0665   0.811 - 1.057   0.980 - 1.155   2.147    5290    4279
    2   12.9  0.0567   0.719 - 0.987   0.973 - 1.107   2.089    2983    2514
    3   12.9  0.0516   0.714 - 1.068   0.968 - 1.144   2.041    2630    2239
Ratio of minimum to maximum apparent transmission: 0.838230

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr AK Croft  
  Local Code   AGSBn  
  Formula   C21H26O9S  
  Crystal Colour    Colourless  
  Crystal Habit    Rod  
  Crystal Size   0.02 x 0.02 x 0.15 (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/