EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2008lsh050

Report generated Jul 18, 2008; 15:27:36

Unit cell

3870 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p222
a (Angstrom)7.6655 +/- 0.0003
b (Angstrom)9.2544 +/- 0.0002
c (Angstrom)10.5957 +/- 0.0003
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)751.65 +/- 0.04
Mosaicity (°)0.375 +/- 0.002

Data collection

Summary

Total number of images collected147
Total exposure time24.6 minutes
Data collection exposure time23.7 minutes
Data collection wall-clock time34.9 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 collections01f84168.0° phi2.000°10 secondsYes
data collections02f55110.0° omega2.000°10 secondsYes
Phi/Chii01f - i08f87 seconds

Scalepack Scaling

Deleted observations

Rejected   6
Overload or incomplete profile 302
Sigma cutoff  14

Final Data Set

Scale factor10.00
Number of 'full' reflections  5665
Number of 'partial' reflections  2156
Total number of integrated reflections  7541
Total number of unique reflections  1019
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  272.6
Average Sigma(I)    4.7
Overall R-merge (linear)  0.072

Sadabs Results

Estimated minimum and maximum transmission: 0.6723 0.7456

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PFA/OMe  
  Formula   C8 H9 N1 O2  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.7 x 0.6 x 0.4 (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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/