EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/07skc0004

Report generated Feb 05, 2007; 12:42:21

Unit cell

3704 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p1
a (Angstrom)5.7680 +/- 0.0009
b (Angstrom)13.704 +/- 0.003
c (Angstrom)14.441 +/- 0.003
alpha (°)89.927 +/- 0.008
beta (°)82.540 +/- 0.011
gamma (°)89.997 +/- 0.009
Volume (A**3)1131.8 +/- 0.4
Mosaicity (°)1.955 +/- 0.007

Data collection

Summary

Total number of images collected226
Total exposure time9.2 hours
Data collection exposure time9.1 hours
Data collection wall-clock time9.2 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f181362.0° phi2.000°150 secondsYes
data collections02f13 26.0° omega2.000°150 secondsYes
data collections03f24 48.0° omega2.000°150 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected 210
Zero sigma or profile test  29
Overload or incomplete profile 670
Sigma cutoff 917
High resolution limit 151

Final Data Set

Scale factor range9.43-12.12
Number of 'full' reflections    48
Number of 'partial' reflections 15363
Total number of integrated reflections 12286
Total number of unique reflections  4844
Data completeness  91.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   15.7
Average Sigma(I)    2.4
Overall R-merge (linear)  0.167

Sadabs Results

Parameter refinement on 5845 reflections reduced R(int) from 0.1361 to 0.0802

Before rejection, 14526 reflections total and 5154 unique

After rejection, 12702 reflections total and 5060 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.1568   0.917 - 1.165   0.917 - 1.279   2.136   10845    4422
    2   11.1  0.0982   0.930 - 1.078   0.944 - 1.320   1.932     585     257
    3   11.1  0.2405   0.247 - 0.303   0.962 - 1.808   2.256    1272     412
Ratio of minimum to maximum apparent transmission: 0.507418

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp8 g7  
  Formula   C8H12O5N1  
  Crystal Colour    Colourless  
  Crystal Habit    Needle  
  Crystal Size   0.18 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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_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. (2003). SADABS. Version 2.10. 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/