EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/04src0553

Report generated Jul 09, 2004; 16:06:38

Unit cell

8772 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)16.8326 +/- 0.0002
b (Angstrom)19.2503 +/- 0.0003
c (Angstrom)22.9949 +/- 0.0004
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)7451.1 +/- 0.2
Mosaicity (°)0.3690 +/- 0.0010

Data collection


Total number of images collected104
Total exposure time39.3 minutes
Data collection exposure time38.8 minutes
Data collection wall-clock time54.0 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f96192.0° phi2.000°24 secondsYes
Phi/Chii01f - i08f84 seconds

Scalepack Scaling

Deleted observations

Rejected 240
Zero sigma or profile test   1
Overload or incomplete profile1632
Sigma cutoff  62
High resolution limit  14

Final Data Set

Scale factor range9.82-10.27
Number of 'full' reflections 35080
Number of 'partial' reflections 12884
Total number of integrated reflections 45313
Total number of unique reflections  9241
Data completeness  99.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   53.9
Average Sigma(I)    1.8
Overall R-merge (linear)  0.039

Sadabs Results

Parameter refinement on 32633 reflections reduced R(int) from 0.0745 to 0.0342

Before rejection, 46370 reflections total and 9264 unique

After rejection, 45408 reflections total and 9252 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0385   0.908 - 0.981   0.949 - 1.183   1.397   45408   33101
Ratio of minimum to maximum apparent transmission: 0.802087


  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Butler  
  Local Code   3-178  
  Formula   C37H58ClFeO4P2Rh  
  Crystal Colour    Orange  
  Crystal Habit    Block  
  Crystal Size   0.35 x 0.3 x 0.25 (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/