EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2010src0796

Report generated Aug 24, 2010; 13:07:36

Unit cell

13752 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)4.1302 +/- 0.0002
b (Angstrom)12.9513 +/- 0.0009
c (Angstrom)13.0829 +/- 0.0009
alpha (°)62.708 +/- 0.003
beta (°)86.496 +/- 0.004
gamma (°)86.546 +/- 0.004
Volume (A**3)620.35 +/- 0.07
Mosaicity (°)0.957 +/- 0.004

Data collection

Summary

Total number of images collected324
Total exposure time109.7 minutes
Data collection exposure time107.0 minutes
Data collection wall-clock time124.7 minutes

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 collections01f176352.0° phi2.000°20 secondsYes
data collections02f24 48.0° omega2.000°20 secondsYes
data collections03f13 26.0° omega2.000°20 secondsYes
data collections04f51102.0° omega2.000°20 secondsYes
data collections05f52104.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Zero sigma or profile test   3
Overload or incomplete profile 378
Sigma cutoff 280
High resolution limit   2

Final Data Set

Scale factor10.00
Number of 'full' reflections  4559
Number of 'partial' reflections  7938
Total number of integrated reflections 11489
Total number of unique reflections  2878
Data completeness  98.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   40.5
Average Sigma(I)    1.7
Overall R-merge (linear)  0.135

Sadabs Results

Parameter refinement on 7507 reflections reduced R(int) from 0.0900 to 0.0507

Before rejection, 11715 reflections total and 2885 unique

After rejection, 10310 reflections total and 2863 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0615   0.765 - 1.045   0.971 - 1.206   2.107    5823    3609
    2   11.1  0.0613   0.801 - 0.865   0.977 - 1.138   2.036     723     476
    3   11.1  0.0540   0.781 - 0.948   0.971 - 1.049   2.076     357     227
    4   11.1  0.0589   0.496 - 0.674   0.977 - 1.118   2.085    1686    1108
    5   11.1  0.0563   0.922 - 1.307   0.971 - 1.085   2.099    1721    1069
Ratio of minimum to maximum apparent transmission: 0.805120

Metadata

  Group    Service  
  Operator   Graham Tizzard  
  Sample Owner   Dr J Spencer  
  Local Code   GRE.Js5  
  Formula   C16H13N1O2  
  Crystal Colour    Yellow  
  Crystal Habit    Plate  
  Crystal Size   0.16 x 0.1 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/