EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: home/ccd/2010sl0004

Report generated Nov 25, 2010; 07:49:31

Unit cell

18079 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)12.8476 +/- 0.0008
b (Angstrom)3.7474 +/- 0.0002
c (Angstrom)21.5262 +/- 0.0014
alpha (°) 90.000
beta (°)97.291 +/- 0.003
gamma (°) 90.000
Volume (A**3)1028.00 +/- 0.11
Mosaicity (°)0.889 +/- 0.003

Data collection

Summary

Total number of images collected281
Total exposure time12.2 hours
Data collection exposure time12.1 hours
Data collection wall-clock time12.5 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 collections01f179286.4° phi1.600°160 secondsYes
data collections02f30 48.0° omega1.600°160 secondsYes
data collections03f64102.4° omega1.600°160 secondsYes
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Rejected  18
Zero sigma or profile test   2
Overload or incomplete profile 532
Sigma cutoff  22

Final Data Set

Scale factor10.00
Number of 'full' reflections  4660
Number of 'partial' reflections 10925
Total number of integrated reflections 13550
Total number of unique reflections  2691
Data completeness  98.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   54.4
Average Sigma(I)    2.5
Overall R-merge (linear)  0.120

Sadabs Results

Estimated minimum and maximum transmission: 0.5176 0.7456

Metadata

  Group    Dr Simon Coles  
  Operator   Sam Ling  
  Sample Owner     
  Local Code   TLT703/3  
  Formula   C13 H8 F3 N1  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.60 x 0.04 x 0.03 (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/