EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2008lsh053

Report generated Jul 20, 2008; 20:18:33

Unit cell

44677 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)27.097 +/- 0.006
b (Angstrom)4.5781 +/- 0.0007
c (Angstrom)9.901 +/- 0.002
alpha (°) 90.000
beta (°)96.281 +/- 0.008
gamma (°) 90.000
Volume (A**3)1220.8 +/- 0.4
Mosaicity (°)3.624 +/- 0.006

Data collection

Summary

Total number of images collected520
Total exposure time8.6 hours
Data collection exposure time8.4 hours
Data collection wall-clock time8.9 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f242363.0° phi1.500°60 secondsYes
data collections02f18 27.0° omega1.500°60 secondsYes
data collections03f36 54.0° omega1.500°60 secondsYes
data collections04f36 54.0° omega1.500°60 secondsYes
data collections05f18 27.0° omega1.500°60 secondsYes
data collections06f48 72.0° omega1.500°60 secondsYes
data collections07f37 55.5° omega1.500°60 secondsYes
data collections08f69103.5° omega1.500°60 secondsYes
Phi/Chii01f - i08f820 seconds
Phi/Chij01f - j08f850 seconds

Scalepack Scaling

Deleted observations

Rejected   3
Zero sigma or profile test   4
Overload or incomplete profile 614
Sigma cutoff 803
High resolution limit  48

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 10024
Total number of integrated reflections  6685
Total number of unique reflections  1470
Data completeness  92.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  181.8
Average Sigma(I)    5.7
Overall R-merge (linear)  0.100

Sadabs Results

Parameter refinement on 7788 reflections reduced R(int) from 0.0999 to 0.0538

Before rejection, 11093 reflections total and 1593 unique

After rejection, 9376 reflections total and 1587 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0542   1.126 - 1.722   0.926 - 1.591   2.111    4644    3013
    2   14.6  0.0641   0.529 - 0.600   1.000 - 1.271   2.236     246     165
    3   14.6  0.0689   0.408 - 0.549   0.941 - 1.306   2.186     666     476
    4   14.6  0.0544   0.490 - 0.541   0.996 - 1.356   2.114     665     469
    5   14.6  0.0526   0.473 - 0.557   0.944 - 1.094   2.096     256     193
    6   14.6  0.0588   0.623 - 0.989   0.941 - 1.245   2.045     884     616
    7   14.6  0.0524   0.290 - 0.333   0.971 - 1.433   1.948     673     503
    8   14.6  0.0632   1.151 - 1.478   0.969 - 1.529   2.094    1342     854
Ratio of minimum to maximum apparent transmission: 0.581843

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PTA/OMe  
  Formula   C9 H8 F3 N1 O2  
  Crystal Colour    Colourless  
  Crystal Habit    Sheet  
  Crystal Size   0.3 x 0.12 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 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/