EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008lsh167

Report generated Jan 08, 2009; 15:45:34

Unit cell

18819 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)7.5138 +/- 0.0005
b (Angstrom)9.3146 +/- 0.0007
c (Angstrom)12.8999 +/- 0.0011
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)902.84 +/- 0.12
Mosaicity (°)1.614 +/- 0.004

Data collection

Summary

Total number of images collected170
Total exposure time111.0 minutes
Data collection exposure time108.8 minutes
Data collection wall-clock time120.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f51102.0° omega2.000°40 secondsYes
data collections02f23 46.0° omega2.000°40 secondsYes
data collections03f41 82.0° omega2.000°40 secondsYes
data collections04f47 94.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f816 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Overload or incomplete profile 646
Sigma cutoff 358
High resolution limit  64

Final Data Set

Scale factor10.00
Number of 'full' reflections   739
Number of 'partial' reflections  9323
Total number of integrated reflections  8386
Total number of unique reflections  1209
Data completeness  98.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  215.0
Average Sigma(I)    5.3
Overall R-merge (linear)  0.232

Sadabs Results

Parameter refinement on 6402 reflections reduced R(int) from 0.1647 to 0.0590

Before rejection, 8744 reflections total and 1224 unique

After rejection, 7477 reflections total and 1217 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.2  0.0919   0.776 - 1.113   0.791 - 1.170   2.272    2447    1477
    2   10.3  0.0455   0.597 - 0.699   0.969 - 1.237   1.942    1010     767
    3   10.2  0.0670   0.802 - 1.344   0.844 - 1.240   2.122    1880    1230
    4   10.2  0.0506   0.589 - 0.778   0.754 - 1.201   1.890    2140    1722
Ratio of minimum to maximum apparent transmission: 0.608369

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PAA/COOMe  
  Formula   C10 H11 N1 O3  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Lath  
  Crystal Size   0.18 x 0.012 x 0.08 (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/