EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008src1284

Report generated Dec 22, 2008; 11:03:23

Unit cell

18603 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)10.2193 +/- 0.0005
b (Angstrom)11.7105 +/- 0.0006
c (Angstrom)13.2331 +/- 0.0006
alpha (°) 90.000
beta (°)99.664 +/- 0.003
gamma (°) 90.000
Volume (A**3)1561.17 +/- 0.13
Mosaicity (°)0.817 +/- 0.003

Data collection

Summary

Total number of images collected202
Total exposure time113.0 minutes
Data collection exposure time110.9 minutes
Data collection wall-clock time124.6 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 collections01f46 92.0° omega2.000°34 secondsYes
data collections02f47 94.0° omega2.000°34 secondsYes
data collections03f50100.0° omega2.000°34 secondsYes
data collections04f51102.0° omega2.000°34 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Overload or incomplete profile 654
Sigma cutoff 528
Low resolution limit   8

Final Data Set

Scale factor10.00
Number of 'full' reflections  8879
Number of 'partial' reflections 11624
Total number of integrated reflections 18712
Total number of unique reflections  3755
Data completeness  98.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   25.8
Average Sigma(I)    1.5
Overall R-merge (linear)  0.179

Sadabs Results

Parameter refinement on 11479 reflections reduced R(int) from 0.1311 to 0.0740

Before rejection, 18932 reflections total and 3766 unique

After rejection, 16239 reflections total and 3734 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.5  0.1081   0.628 - 0.837   0.994 - 1.061   2.058    3923    2249
    2   10.2  0.1037   0.974 - 1.329   0.976 - 1.092   2.057    3923    2206
    3   10.2  0.0983   0.863 - 1.187   0.976 - 1.110   2.042    4163    2499
    4   10.2  0.0992   0.548 - 0.880   0.965 - 1.850   2.033    4230    2527
Ratio of minimum to maximum apparent transmission: 0.521566

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   HP132(7)  
  Formula   C9H14N4O2S  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.07 x 0.02 x 0.01 (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/