EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04src1115

Report generated Dec 02, 2004; 13:51:09

Unit cell

7246 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)15.4637 +/- 0.0007
b (Angstrom)11.6125 +/- 0.0005
c (Angstrom)20.5526 +/- 0.0009
alpha (°) 90.000
beta (°)107.713 +/- 0.002
gamma (°) 90.000
Volume (A**3)3515.7 +/- 0.3
Mosaicity (°)1.410 +/- 0.002

Data collection


Total number of images collected264
Total exposure time130.3 minutes
Data collection exposure time128.9 minutes
Data collection wall-clock time149.1 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance40.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f131262.0° phi2.000°30 secondsYes
data collections02f64128.0° omega2.000°30 secondsYes
data collections03f61122.0° omega2.000°30 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test   2
Overload or incomplete profile2486
Sigma cutoff 131
High resolution limit 345

Final Data Set

Scale factor range8.50-10.27
Number of 'full' reflections  6692
Number of 'partial' reflections 35071
Total number of integrated reflections 34529
Total number of unique reflections  8022
Data completeness  95.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   64.9
Average Sigma(I)    3.7
Overall R-merge (linear)  0.091

Sadabs Results

Parameter refinement on 26402 reflections reduced R(int) from 0.1773 to 0.0907

Before rejection, 41085 reflections total and 8341 unique

After rejection, 38787 reflections total and 8331 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.1065   0.754 - 0.966   0.945 - 1.458   1.469   19142   13239
    2  -15.0  0.1231   0.849 - 0.988   0.946 - 1.249   1.484   10424    6590
    3  -15.0  0.1103   0.730 - 0.968   0.944 - 1.220   1.506    9221    6099
Ratio of minimum to maximum apparent transmission: 0.647447


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. C. J. Matthews  
  Local Code   LJD459Zn  
  Formula   C72 H66 N36 O32 Cl8 Zn4  
  Crystal Colour    Yellow  
  Crystal Habit    Plate  
  Crystal Size   0.16 x 0.14 x 0.03 (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    '10cm confocal mirrors'
_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/