EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04src0550

Report generated Jul 13, 2004; 11:03:11

Unit cell

7711 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)11.5454 +/- 0.0003
b (Angstrom)14.4162 +/- 0.0003
c (Angstrom)20.5192 +/- 0.0005
alpha (°) 90.000
beta (°)95.4090 +/- 0.0015
gamma (°) 90.000
Volume (A**3)3400.02 +/- 0.14
Mosaicity (°)0.3540 +/- 0.0010

Data collection


Total number of images collected180
Total exposure time59.1 minutes
Data collection exposure time58.0 minutes
Data collection wall-clock time74.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f133266.0° phi2.000°20 secondsYes
data collections02f39 78.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected 173
Zero sigma or profile test   6
Overload or incomplete profile 832
Sigma cutoff   2
High resolution limit  18

Final Data Set

Scale factor range9.95-10.37
Number of 'full' reflections 26181
Number of 'partial' reflections  9023
Total number of integrated reflections 34076
Total number of unique reflections  8074
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   16.4
Average Sigma(I)    1.1
Overall R-merge (linear)  0.060

Sadabs Results

Parameter refinement on 22094 reflections reduced R(int) from 0.0626 to 0.0446

Before rejection, 34057 reflections total and 8094 unique

After rejection, 33765 reflections total and 8089 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0575   1.016 - 1.178   0.932 - 1.147   1.233   26328   18476
    2  -11.2  0.0572   0.631 - 0.677   0.940 - 1.155   1.192    7437    5357
Ratio of minimum to maximum apparent transmission: 0.806683


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. Ian Butler  
  Local Code   IRBKM20  
  Formula   C28 H48 P2 Fe1 Pd1 Cl2  
  Crystal Colour    Orange  
  Crystal Habit    Shard  
  Crystal Size   0.32 x 0.26 x 0.1 (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. 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/