EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005slh0428

Report generated May 08, 2005; 20:12:29

Unit cell

3111 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)10.2942 +/- 0.0004
b (Angstrom)29.7386 +/- 0.0014
c (Angstrom)9.2931 +/- 0.0004
alpha (°) 90.000
beta (°)90.374 +/- 0.003
gamma (°) 90.000
Volume (A**3)2844.9 +/- 0.2
Mosaicity (°)1.582 +/- 0.002

Data collection


Total number of images collected364
Total exposure time61.9 minutes
Data collection exposure time60.6 minutes
Data collection wall-clock time91.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f302302.0° phi1.000°10 secondsYes
data collections02f54 54.0° omega1.000°10 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 273
Zero sigma or profile test   7
Overload or incomplete profile 816
Sigma cutoff  14

Final Data Set

Scale factor range10.00-13.59
Number of 'full' reflections     0
Number of 'partial' reflections 14572
Total number of integrated reflections 13437
Total number of unique reflections  3308
Data completeness  99.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  238.8
Average Sigma(I)    6.1
Overall R-merge (linear)  0.038

Sadabs Results

Parameter refinement on 13212 reflections reduced R(int) from 0.0750 to 0.0372

Before rejection, 14636 reflections total and 3333 unique

After rejection, 14429 reflections total and 3332 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0369   0.751 - 1.060   0.914 - 1.365   1.507   12235   11232
    2  -11.2  0.0417   0.913 - 1.033   0.951 - 1.258   1.675    2194    1996
Ratio of minimum to maximum apparent transmission: 0.669645


  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 153  
  Formula   C46 H54 N4 O4 P2 S4 Ni1 Pt1  
  Crystal Colour    Green  
  Crystal Habit    Slab  
  Crystal Size   0.2 x 0.1 x 0.04 (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. (2003). SADABS. Version 2.10. 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/