EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005slh0246

Report generated Apr 02, 2005; 12:51:35

Unit cell

2500 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)10.9250 +/- 0.0002
b (Angstrom)11.90410 +/- 0.00010
c (Angstrom)14.8990 +/- 0.0003
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1937.65 +/- 0.06
Mosaicity (°)0.4840 +/- 0.0010

Data collection


Total number of images collected329
Total exposure time28.6 minutes
Data collection exposure time27.9 minutes
Data collection wall-clock time58.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f263263.0° phi1.000°5 secondsYes
data collections02f58 58.0° omega1.000°5 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 256
Zero sigma or profile test   3
Overload or incomplete profile 774
Sigma cutoff  27
High resolution limit   4

Final Data Set

Scale factor range8.78-10.22
Number of 'full' reflections  8244
Number of 'partial' reflections 14448
Total number of integrated reflections 20883
Total number of unique reflections  2534
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   97.6
Average Sigma(I)    2.2
Overall R-merge (linear)  0.048

Sadabs Results

Parameter refinement on 19409 reflections reduced R(int) from 0.0883 to 0.0409

Before rejection, 22303 reflections total and 2539 unique

After rejection, 21904 reflections total and 2538 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0415   0.940 - 1.167   0.801 - 1.329   1.534   18035   15771
    2   -6.8  0.0418   0.558 - 0.617   0.807 - 1.329   1.471    3869    3421
Ratio of minimum to maximum apparent transmission: 0.602577


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 129  
  Formula   C13 H12 N6 I1 Br1  
  Crystal Colour    Orange  
  Crystal Habit    Block  
  Crystal Size   0.6 x 0.46 x 0.25 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

      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

'COLLECT (Hooft, R.W.W., 1998)'
'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
'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/