EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008lsh121

Report generated Nov 08, 2008; 19:42:59

Unit cell

4372 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)20.8029 +/- 0.0013
b (Angstrom)4.7163 +/- 0.0003
c (Angstrom)6.7095 +/- 0.0003
alpha (°) 90.000
beta (°)105.889 +/- 0.004
gamma (°) 90.000
Volume (A**3)633.14 +/- 0.06
Mosaicity (°)0.757 +/- 0.004

Data collection

Summary

Total number of images collected209
Total exposure time274.4 minutes
Data collection exposure time269.1 minutes
Data collection wall-clock time281.9 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°80 secondsYes
data collections02f51102.0° omega2.000°80 secondsYes
data collections03f51102.0° omega2.000°80 secondsYes
data collections04f48 96.0° omega2.000°80 secondsYes
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test   1
Overload or incomplete profile 118
Sigma cutoff  38
High resolution limit  29

Final Data Set

Scale factor10.00
Number of 'full' reflections  2032
Number of 'partial' reflections  2258
Total number of integrated reflections  4030
Total number of unique reflections   802
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  198.7
Average Sigma(I)    4.5
Overall R-merge (linear)  0.135

Sadabs Results

Parameter refinement on 3554 reflections reduced R(int) from 0.1307 to 0.0423

Before rejection, 3984 reflections total and 811 unique

After rejection, 3631 reflections total and 808 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.1  0.0444   0.904 - 1.549   0.880 - 1.069   2.276     939     831
    2   10.2  0.0421   0.379 - 0.650   0.877 - 1.079   2.069     916     827
    3   10.2  0.0412   0.904 - 1.715   0.922 - 1.152   2.173     906     800
    4   10.2  0.0394   0.982 - 1.449   0.984 - 1.155   2.089     870     760
Ratio of minimum to maximum apparent transmission: 0.759853

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   MMC/NO2  
  Formula   C8 H8 N2 O3  
  Crystal Colour    Colourless  
  Crystal Habit    Needle  
  Crystal Size   0.44 x 0.02 x 0.01 (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/