EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2007src0866

Report generated Jul 10, 2007; 07:15:39

Unit cell

4477 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)6.5148 +/- 0.0003
b (Angstrom)11.4581 +/- 0.0005
c (Angstrom)6.8511 +/- 0.0002
alpha (°) 90.000
beta (°)111.601 +/- 0.002
gamma (°) 90.000
Volume (A**3)475.50 +/- 0.03
Mosaicity (°)0.487 +/- 0.003

Data collection


Total number of images collected195
Total exposure time12.6 hours
Data collection exposure time12.5 hours
Data collection wall-clock time12.7 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f116232.0° phi2.000°240 secondsYes
data collections02f23 46.0° omega2.000°240 secondsYes
data collections03f48 96.0° omega2.000°240 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected   5
Overload or incomplete profile 120
Sigma cutoff   4

Final Data Set

Scale factor10.00
Number of 'full' reflections  4262
Number of 'partial' reflections  2358
Total number of integrated reflections  6373
Total number of unique reflections  1151
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  181.4
Average Sigma(I)    4.8
Overall R-merge (linear)  0.048

Sadabs Results

Estimated minimum and maximum transmission: 0.6606 0.7456


  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr PJ Holliman  
  Local Code   AcPdCN  
  Formula   C12 H8 N2 Pd1 Cl2 Fe1  
  Crystal Colour    Orange  
  Crystal Habit    Plate  
  Crystal Size   0.13 x 0.07 x 0.2 (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 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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/