EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2005slh1128

Report generated Sep 29, 2005; 13:00:28

Unit cell

7252 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p1
a (Angstrom)9.8837 +/- 0.0002
b (Angstrom)11.8446 +/- 0.0003
c (Angstrom)14.5108 +/- 0.0003
alpha (°)104.0099 +/- 0.0011
beta (°)95.5232 +/- 0.0014
gamma (°)98.0781 +/- 0.0012
Volume (A**3)1616.80 +/- 0.06
Mosaicity (°)0.6260 +/- 0.0010

Data collection

Summary

Total number of images collected301
Total exposure time100.1 minutes
Data collection exposure time98.7 minutes
Data collection wall-clock time123.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f181362.0° phi2.000°20 secondsYes
data collections02f17 34.0° omega2.000°20 secondsYes
data collections03f17 34.0° omega2.000°20 secondsYes
data collections04f55110.0° omega2.000°20 secondsYes
data collections05f23 46.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 199
Zero sigma or profile test   3
Overload or incomplete profile1226
Sigma cutoff  35
High resolution limit 116

Final Data Set

Scale factor range9.19-10.10
Number of 'full' reflections 19606
Number of 'partial' reflections 15359
Total number of integrated reflections 33412
Total number of unique reflections  7364
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  209.0
Average Sigma(I)    4.8
Overall R-merge (linear)  0.045

Sadabs Results

Parameter refinement on 27916 reflections reduced R(int) from 0.0708 to 0.0439

Before rejection, 32976 reflections total and 7413 unique

After rejection, 32586 reflections total and 7410 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0425   0.947 - 1.066   0.941 - 1.183   1.359   20565   17977
    2   -6.8  0.0473   0.753 - 0.813   0.941 - 1.048   1.373    1710    1510
    3   -6.8  0.0414   0.691 - 0.720   0.964 - 1.086   1.371    1714    1470
    4   -6.8  0.0460   0.900 - 0.980   0.943 - 1.086   1.361    6178    5315
    5   -6.8  0.0499   0.756 - 0.814   0.941 - 1.093   1.406    2419    2065
Ratio of minimum to maximum apparent transmission: 0.795380

Metadata

  Group    Personal  
  Operator   Mike Hursthouse  
  Sample Owner   SLH/CAG  
  Local Code   CAG161  
  Formula   C28H32N2O4P2S4Cd1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.3 x 0.2 x 0.2 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      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

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'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
_computing_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/