EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0075

Report generated Nov 26, 2006; 07:50:10

Unit cell

5583 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)10.0641 +/- 0.0008
b (Angstrom)10.7251 +/- 0.0007
c (Angstrom)12.7628 +/- 0.0010
alpha (°)90.565 +/- 0.005
beta (°)105.919 +/- 0.004
gamma (°)99.929 +/- 0.005
Volume (A**3)1302.55 +/- 0.17
Mosaicity (°)2.271 +/- 0.004

Data collection

Summary

Total number of images collected620
Total exposure time12.4 hours
Data collection exposure time12.3 hours
Data collection wall-clock time12.8 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°72 secondsYes
data collections02f13 26.0° omega2.000°72 secondsYes
data collections03f27 54.0° omega2.000°72 secondsYes
data collections04f27 54.0° omega2.000°72 secondsYes
data collections05f55110.0° omega2.000°72 secondsYes
data collections06f28 56.0° omega2.000°72 secondsYes
data collections07f55110.0° omega2.000°72 secondsYes
data collections08f55110.0° omega2.000°72 secondsYes
data collections09f27 54.0° omega2.000°72 secondsYes
data collections10f56112.0° omega2.000°72 secondsNo
data collections11f50100.0° omega2.000°72 secondsNo
data collections12f38 76.0° omega2.000°72 secondsNo
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 958
Zero sigma or profile test  29
Overload or incomplete profile1188
Sigma cutoff1157
High resolution limit 468

Final Data Set

Scale factor range2.40-15.60
Number of 'full' reflections     0
Number of 'partial' reflections 28742
Total number of integrated reflections 22503
Total number of unique reflections  5871
Data completeness  98.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   37.7
Average Sigma(I)    2.2
Overall R-merge (linear)  0.143

Sadabs Results

Parameter refinement on 26120 reflections reduced R(int) from 0.1957 to 0.0971

Before rejection, 40213 reflections total and 6136 unique

After rejection, 33645 reflections total and 6121 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0842   0.694 - 1.013   0.970 - 1.215   1.932   10269    6982
    2   14.6  0.0832   0.779 - 0.876   1.014 - 1.194   1.895     584     421
    3   14.6  0.1357   0.334 - 0.383   0.970 - 1.285   2.160    1421     797
    4   14.6  0.3491   1.268 - 1.896   1.011 - 1.312   2.327    1343     398
    5   14.6  0.0697   0.716 - 0.941   0.971 - 1.303   1.764    3018    2322
    6   14.6  0.1114   0.411 - 0.586   0.986 - 1.250   2.124    1513     925
    7   14.6  0.1437   0.586 - 1.229   0.985 - 1.313   2.135    3090    1633
    8   14.6  0.1112   0.707 - 1.326   0.981 - 1.314   1.930    3033    2133
    9   14.6  0.2743   0.439 - 0.626   0.992 - 1.312   2.197    1400     525
   10   14.6  0.1534   0.602 - 1.468   0.985 - 1.315   2.126    3013    1619
   11   14.6  0.0895   0.591 - 0.829   0.971 - 1.285   1.899    2833    2015
   12   14.6  0.1890   0.647 - 1.010   0.971 - 1.315   2.132    2128     985
Ratio of minimum to maximum apparent transmission: 0.737422

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp15 a2  
  Formula   C11H17O3N1S1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.14 x 0.09 x 0.02 (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    '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

_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/