EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04src0437r

Report generated Jun 07, 2004; 11:48:46

Unit cell

13812 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)19.5018 +/- 0.0004
b (Angstrom)11.1612 +/- 0.0002
c (Angstrom)30.3744 +/- 0.0006
alpha (°) 90.000
beta (°)91.5624 +/- 0.0006
gamma (°) 90.000
Volume (A**3)6608.9 +/- 0.2
Mosaicity (°)0.4130 +/- 0.0010

Data collection


Total number of images collected580
Total exposure time79.0 minutes
Data collection exposure time78.3 minutes
Data collection wall-clock time132.0 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance55.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f377301.6° phi0.800°8 secondsYes
data collections02f195156.0° omega0.800°8 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 305
Zero sigma or profile test   6
Overload or incomplete profile1980
Sigma cutoff   8
High resolution limit  35

Final Data Set

Scale factor range9.08-12.38
Number of 'full' reflections 19647
Number of 'partial' reflections 32732
Total number of integrated reflections 44953
Total number of unique reflections 15512
Data completeness  97.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   87.5
Average Sigma(I)    3.3
Overall R-merge (linear)  0.034

Sadabs Results

Parameter refinement on 38565 reflections reduced R(int) from 0.0880 to 0.0338

Before rejection, 51431 reflections total and 15770 unique

After rejection, 50486 reflections total and 15744 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   24.2  0.0322   0.844 - 1.186   0.931 - 1.188   1.287   33134   26374
    2  -23.6  0.0378   0.792 - 0.969   0.939 - 1.135   1.351   17352   13518
Ratio of minimum to maximum apparent transmission: 0.784008


  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. Ian Butler  
  Local Code   6-163  
  Formula   C30 H52 Cl2 Fe1 P2 Pd1  
  Crystal Colour    Red  
  Crystal Habit    Slab  
  Crystal Size   0.56 x 0.4 x 0.16 (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/