EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/06skc0013

Report generated Mar 18, 2006; 19:23:45

Unit cell

3149 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)8.8691 +/- 0.0007
b (Angstrom)13.2988 +/- 0.0017
c (Angstrom)12.1250 +/- 0.0014
alpha (°) 90.000
beta (°)109.500 +/- 0.007
gamma (°) 90.000
Volume (A**3)1348.1 +/- 0.3
Mosaicity (°)1.416 +/- 0.005

Data collection

Summary

Total number of images collected258
Total exposure time254.9 minutes
Data collection exposure time250.9 minutes
Data collection wall-clock time272.3 minutes

Experimental Conditions

Wavelength0.71073 A
Cryostat setting120.00K
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f178356.0° phi2.000°60 secondsYes
data collections02f29 58.0° omega2.000°60 secondsYes
data collections03f27 54.0° omega2.000°60 secondsYes
data collections04f16 32.0° omega2.000°60 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 210
Zero sigma or profile test  49
Overload or incomplete profile1070
Sigma cutoff  70
High resolution limit  31

Final Data Set

Scale factor range4.04-10.99
Number of 'full' reflections  3066
Number of 'partial' reflections 17587
Total number of integrated reflections 19375
Total number of unique reflections  3219
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   13.7
Average Sigma(I)    1.6
Overall R-merge (linear)  0.180

Sadabs Results

Parameter refinement on 7541 reflections reduced R(int) from 0.1230 to 0.0757

Before rejection, 18941 reflections total and 3234 unique

After rejection, 18518 reflections total and 3234 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.1514   1.014 - 1.556   0.931 - 1.239   1.384   13486    6214
    2   -4.9  0.1430   0.337 - 0.368   0.931 - 1.215   1.355    2120    1103
    3  -11.2  0.3708   1.267 - 1.697   0.944 - 1.192   1.539    1866     498
    4  -11.2  0.1695   0.292 - 0.324   0.932 - 1.205   1.366    1046     469
Ratio of minimum to maximum apparent transmission: 0.751479

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp5 c6  
  Formula   C12H18O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Shard  
  Crystal Size   0.1 x 0.07 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/