EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008lsh018

Report generated Jul 05, 2008; 14:05:35

Unit cell

12717 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)9.2804 +/- 0.0002
b (Angstrom)9.3819 +/- 0.0002
c (Angstrom)20.7436 +/- 0.0005
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1806.10 +/- 0.07
Mosaicity (°)0.4810 +/- 0.0010

Data collection

Summary

Total number of images collected192
Total exposure time26.2 minutes
Data collection exposure time25.5 minutes
Data collection wall-clock time33.2 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 collections01f56 89.6° omega1.600°8 secondsYes
data collections02f38 60.8° omega1.600°8 secondsYes
data collections03f61 97.6° omega1.600°8 secondsYes
data collections04f29 46.4° omega1.600°8 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected   4
Overload or incomplete profile 926
Sigma cutoff 262
High resolution limit  42

Final Data Set

Scale factor10.00
Number of 'full' reflections 10276
Number of 'partial' reflections  7768
Total number of integrated reflections 16536
Total number of unique reflections  2361
Data completeness  99.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  366.0
Average Sigma(I)    6.4
Overall R-merge (linear)  0.131

Sadabs Results

Parameter refinement on 12504 reflections reduced R(int) from 0.1040 to 0.0329

Before rejection, 16543 reflections total and 2376 unique

After rejection, 14951 reflections total and 2372 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.4  0.0331   0.909 - 1.116   0.923 - 1.640   2.179    4696    3561
    2    8.8  0.0372   0.814 - 1.136   0.923 - 1.654   2.210    3059    2254
    3   -7.9  0.0309   0.689 - 0.963   0.923 - 1.582   2.087    4966    3692
    4   10.2  0.0349   0.819 - 0.898   0.929 - 1.457   2.172    2230    1647
Ratio of minimum to maximum apparent transmission: 0.557974

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   PPA/Br  
  Formula   C9 H10 Br1 N1 O1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Needle  
  Crystal Size   0.4 x 0.1 x 0.1 (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/