EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2010src0401

Report generated May 21, 2010; 14:16:37

Unit cell

35554 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)7.3738 +/- 0.0004
b (Angstrom)24.541 +/- 0.002
c (Angstrom)21.2954 +/- 0.0016
alpha (°) 90.000
beta (°)97.475 +/- 0.004
gamma (°) 90.000
Volume (A**3)3820.8 +/- 0.5
Mosaicity (°)1.198 +/- 0.003

Data collection

Summary

Total number of images collected235
Total exposure time268.8 minutes
Data collection exposure time266.0 minutes
Data collection wall-clock time286.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance39.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f126252.0° phi2.000°70 secondsYes
data collections02f13 26.0° omega2.000°70 secondsYes
data collections03f31 62.0° omega2.000°70 secondsYes
data collections04f57114.0° omega2.000°70 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected   7
Zero sigma or profile test  28
Overload or incomplete profile1012
Sigma cutoff1310
Low resolution limit  11
High resolution limit 137

Final Data Set

Scale factor10.00
Number of 'full' reflections  9092
Number of 'partial' reflections 24803
Total number of integrated reflections 23739
Total number of unique reflections  7822
Data completeness  87.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   18.5
Average Sigma(I)    2.3
Overall R-merge (linear)  0.209

Sadabs Results

Parameter refinement on 15881 reflections reduced R(int) from 0.1358 to 0.0778

Before rejection, 32228 reflections total and 8691 unique

After rejection, 27069 reflections total and 8534 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.2  0.1352   0.834 - 1.096   0.960 - 1.154   2.124   15978    7654
    2   17.6  0.1056   0.414 - 0.456   0.956 - 1.190   2.166     853     484
    3   17.6  0.1068   0.417 - 0.512   0.952 - 1.113   2.085    3314    1663
    4   17.6  0.1282   0.954 - 1.544   0.956 - 1.341   2.068    6924    3278
Ratio of minimum to maximum apparent transmission: 0.710015

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr J Spencer  
  Local Code   JA61  
  Formula   C18 H16 N2 O3 S Fe  
  Crystal Colour    Orange  
  Crystal Habit    Needle  
  Crystal Size   0.26 x 0.02 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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/