EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008lsh023

Report generated Jul 05, 2008; 19:04:16

Unit cell

10393 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)7.4415 +/- 0.0003
b (Angstrom)9.5769 +/- 0.0004
c (Angstrom)13.8770 +/- 0.0004
alpha (°) 90.000
beta (°)103.022 +/- 0.002
gamma (°) 90.000
Volume (A**3)963.53 +/- 0.06
Mosaicity (°)0.600 +/- 0.002

Data collection

Summary

Total number of images collected225
Total exposure time74.9 minutes
Data collection exposure time73.5 minutes
Data collection wall-clock time82.8 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 collections01f50100.0° omega2.000°20 secondsYes
data collections02f50100.0° omega2.000°20 secondsYes
data collections03f35 70.0° omega2.000°20 secondsYes
data collections04f48 96.0° omega2.000°20 secondsYes
data collections05f34 68.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Overload or incomplete profile 566
Sigma cutoff 275

Final Data Set

Scale factor10.00
Number of 'full' reflections  8115
Number of 'partial' reflections  6152
Total number of integrated reflections 13258
Total number of unique reflections  2339
Data completeness  98.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  103.1
Average Sigma(I)    2.5
Overall R-merge (linear)  0.190

Sadabs Results

Parameter refinement on 9547 reflections reduced R(int) from 0.1789 to 0.0554

Before rejection, 13110 reflections total and 2340 unique

After rejection, 11374 reflections total and 2325 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.0  0.0634   0.490 - 0.818   0.951 - 1.260   2.216    2714    1993
    2    7.0  0.0527   0.785 - 1.632   0.953 - 1.303   2.077    2564    1820
    3   10.2  0.0516   0.725 - 1.201   0.982 - 1.207   2.147    1813    1253
    4   10.2  0.0458   0.820 - 1.003   0.948 - 1.079   2.041    2524    1774
    5   10.2  0.0463   0.648 - 0.847   0.948 - 1.242   1.981    1759    1321
Ratio of minimum to maximum apparent transmission: 0.727389

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PAA/OH  
  Formula   C8 H9 N1 O2  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Sheet  
  Crystal Size   0.4 x 0.24 x 0.02 (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/