EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/07skc0005

Report generated Feb 08, 2007; 10:50:49

Unit cell

20712 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)5.3007 +/- 0.0004
b (Angstrom)19.374 +/- 0.002
c (Angstrom)10.0779 +/- 0.0010
alpha (°) 90.000
beta (°)94.013 +/- 0.006
gamma (°) 90.000
Volume (A**3)1032.40 +/- 0.17
Mosaicity (°)1.900 +/- 0.005

Data collection

Summary

Total number of images collected260
Total exposure time111.5 minutes
Data collection exposure time110.1 minutes
Data collection wall-clock time130.8 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 collections01f160320.0° phi2.000°26 secondsYes
data collections02f23 46.0° omega2.000°26 secondsYes
data collections03f16 32.0° omega2.000°26 secondsYes
data collections04f53106.0° omega2.000°26 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected  51
Overload or incomplete profile 360
Sigma cutoff  37
High resolution limit  28

Final Data Set

Scale factor range10.00-10.75
Number of 'full' reflections   103
Number of 'partial' reflections  9541
Total number of integrated reflections  8797
Total number of unique reflections  1217
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   75.8
Average Sigma(I)    2.3
Overall R-merge (linear)  0.057

Sadabs Results

Parameter refinement on 6423 reflections reduced R(int) from 0.0700 to 0.0468

Before rejection, 9040 reflections total and 1226 unique

After rejection, 8927 reflections total and 1226 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0549   0.993 - 1.139   0.947 - 1.220   1.237    5797    4400
    2    6.8  0.0605   0.450 - 0.477   0.946 - 1.207   1.270     746     545
    3    6.8  0.0620   0.447 - 0.476   0.946 - 1.116   1.339     484     352
    4    6.8  0.0583   0.987 - 1.081   0.946 - 1.134   1.204    1900    1482
Ratio of minimum to maximum apparent transmission: 0.775264

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 h4  
  Formula   C8H12O5N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.25 x 0.2 x 0.09 (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    'graphite'
_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/