EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/04src0422

Report generated May 27, 2004; 15:50:19

Unit cell

8423 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)23.4352 +/- 0.0010
b (Angstrom)18.0929 +/- 0.0009
c (Angstrom)20.9394 +/- 0.0009
alpha (°) 90.000
beta (°)118.729 +/- 0.002
gamma (°) 90.000
Volume (A**3)7785.6 +/- 0.6
Mosaicity (°)1.193 +/- 0.002

Data collection


Total number of images collected191
Total exposure time62.8 minutes
Data collection exposure time61.7 minutes
Data collection wall-clock time76.2 minutes

Experimental Conditions

Wavelength0.71073 A
Cryostat setting120.00K
Crystal to detector distance40.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f141282.0° phi2.000°20 secondsYes
data collections02f42 84.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 299
Overload or incomplete profile1522
Sigma cutoff  97
High resolution limit  87

Final Data Set

Scale factor range7.65-10.00
Number of 'full' reflections  9139
Number of 'partial' reflections 27099
Total number of integrated reflections 33199
Total number of unique reflections  8995
Data completeness  97.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   79.7
Average Sigma(I)    4.2
Overall R-merge (linear)  0.066

Sadabs Results

Parameter refinement on 21187 reflections reduced R(int) from 0.1714 to 0.0514

Before rejection, 34431 reflections total and 9237 unique

After rejection, 33556 reflections total and 9227 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0605   0.815 - 1.166   0.928 - 1.315   1.458   25783   16986
    2  -15.0  0.0763   0.631 - 0.796   0.978 - 1.316   1.517    7773    4912
Ratio of minimum to maximum apparent transmission: 0.705540


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr Craig Matthews  
  Local Code   LJD394Zn  
  Formula   C87 H75 N39 O24 Cl6 Zn3  
  Crystal Colour   Light Green  
  Crystal Habit    Slab  
  Crystal Size   0.22 x 0.2 x 0.07 (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. SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10

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/