EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2010src0794

Report generated Aug 24, 2010; 07:41:58

Unit cell

17573 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)9.9484 +/- 0.0011
b (Angstrom)7.9134 +/- 0.0010
c (Angstrom)16.013 +/- 0.002
alpha (°) 90.000
beta (°)104.340 +/- 0.008
gamma (°) 90.000
Volume (A**3)1221.4 +/- 0.3
Mosaicity (°)2.361 +/- 0.006

Data collection

Summary

Total number of images collected125
Total exposure time202.3 minutes
Data collection exposure time195.6 minutes
Data collection wall-clock time6.0 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f5 10.0° phi2.000°100 secondsYes
data collections02f13 26.0° omega2.000°100 secondsYes
data collections03f51102.0° omega2.000°100 secondsYes
data collections04f48 96.0° omega2.000°100 secondsYes
Phi/Chii01f - i08f850 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Overload or incomplete profile 434
Sigma cutoff 388
High resolution limit   3

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections  8187
Total number of integrated reflections  5753
Total number of unique reflections  2538
Data completeness  84.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  141.7
Average Sigma(I)    7.0
Overall R-merge (linear)  0.093

Sadabs Results

Parameter refinement on 4620 reflections reduced R(int) from 0.1127 to 0.0502

Before rejection, 7569 reflections total and 2859 unique

After rejection, 6679 reflections total and 2808 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0695   0.843 - 0.895   0.947 - 1.400   1.960     103      72
    2   11.1  0.0615   0.324 - 0.354   0.818 - 1.135   2.126     627     419
    3   11.1  0.0538   1.195 - 1.920   0.928 - 1.603   2.209    3019    2032
    4   11.1  0.0600   0.757 - 0.958   0.928 - 1.306   2.250    2930    1845
Ratio of minimum to maximum apparent transmission: 0.510295

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr J Spencer  
  Local Code   GRE.Js3  
  Formula   C15H10N2O3  
  Crystal Colour    Yellow  
  Crystal Habit    Plate  
  Crystal Size   0.16 x 0.14 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/