EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2005slh0248

Report generated Apr 02, 2005; 18:48:36

Unit cell

8008 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p1
a (Angstrom)8.1475 +/- 0.0003
b (Angstrom)14.0961 +/- 0.0008
c (Angstrom)16.3605 +/- 0.0009
alpha (°)90.925 +/- 0.002
beta (°)99.315 +/- 0.003
gamma (°)100.887 +/- 0.003
Volume (A**3)1818.71 +/- 0.16
Mosaicity (°)0.900 +/- 0.002

Data collection

Summary

Total number of images collected301
Total exposure time199.1 minutes
Data collection exposure time196.4 minutes
Data collection wall-clock time220.2 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 collections01f181362.0° phi2.000°40 secondsYes
data collections02f17 34.0° omega2.000°40 secondsYes
data collections03f17 34.0° omega2.000°40 secondsYes
data collections04f55110.0° omega2.000°40 secondsYes
data collections05f23 46.0° omega2.000°40 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 145
Zero sigma or profile test  12
Overload or incomplete profile1200
Sigma cutoff  43
High resolution limit  95

Final Data Set

Scale factor range9.24-12.42
Number of 'full' reflections 15652
Number of 'partial' reflections 23870
Total number of integrated reflections 36786
Total number of unique reflections  8255
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   12.8
Average Sigma(I)    1.1
Overall R-merge (linear)  0.090

Sadabs Results

Parameter refinement on 18903 reflections reduced R(int) from 0.0759 to 0.0507

Before rejection, 37160 reflections total and 8332 unique

After rejection, 36794 reflections total and 8328 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0853   0.768 - 1.026   0.878 - 1.345   1.248   23388   13327
    2   -6.8  0.0907   0.755 - 0.806   0.879 - 1.306   1.255    1917    1108
    3   -6.8  0.0834   0.877 - 0.950   0.872 - 1.285   1.201    1893    1132
    4   -6.8  0.0864   0.943 - 1.036   0.871 - 1.388   1.219    6892    3979
    5   -6.8  0.0911   0.786 - 0.884   0.885 - 1.382   1.232    2704    1496
Ratio of minimum to maximum apparent transmission: 0.627645

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 130  
  Formula   C13 H12 N6 I1 Br1  
  Crystal Colour    Orange  
  Crystal Habit   Cut Needle  
  Crystal Size   0.46 x 0.04 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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm 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. (2003). SADABS. Version 2.10. 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/