EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0065

Report generated Nov 06, 2006; 13:25:49

Unit cell

6289 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)17.309 +/- 0.002
b (Angstrom)9.0086 +/- 0.0013
c (Angstrom)18.935 +/- 0.002
alpha (°) 90.000
beta (°)105.314 +/- 0.007
gamma (°) 90.000
Volume (A**3)2847.7 +/- 0.6
Mosaicity (°)1.954 +/- 0.006

Data collection

Summary

Total number of images collected359
Total exposure time9.8 hours
Data collection exposure time9.8 hours
Data collection wall-clock time10.2 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°100 secondsYes
data collections02f17 34.0° omega2.000°100 secondsYes
data collections03f16 32.0° omega2.000°100 secondsYes
data collections04f25 50.0° omega2.000°100 secondsYes
data collections05f57114.0° omega2.000°100 secondsYes
data collections06f55110.0° omega2.000°100 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 337
Zero sigma or profile test1056
Overload or incomplete profile3484
Sigma cutoff1278
High resolution limit1641

Final Data Set

Scale factor range9.16-15.48
Number of 'full' reflections   161
Number of 'partial' reflections 58117
Total number of integrated reflections 43840
Total number of unique reflections  6626
Data completeness  97.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity    4.8
Average Sigma(I)    1.4
Overall R-merge (linear)  0.184

Sadabs Results

Parameter refinement on 7530 reflections reduced R(int) from 0.1313 to 0.0725

Before rejection, 54460 reflections total and 6990 unique

After rejection, 53588 reflections total and 6984 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.3466   0.874 - 1.175   0.912 - 1.723   1.184   27920    5646
    2   -8.7  0.5527   0.944 - 1.057   0.909 - 1.816   1.179    2520     407
    3   -8.7  0.3699   0.349 - 0.417   0.927 - 1.128   1.165    1840     362
    4   -8.7  0.4266   0.768 - 0.929   0.903 - 1.828   1.192    4021     827
    5   -8.7  0.3549   0.452 - 0.676   0.896 - 1.200   1.204    7680    1608
    6   -8.7  0.4063   0.790 - 0.990   0.892 - 1.741   1.175    9607    1797
Ratio of minimum to maximum apparent transmission: 0.488335

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 g4  
  Formula   C11H24O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.18 x 0.11 x 0.07 (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    'graphite'
_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/