EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0064

Report generated Nov 03, 2006; 09:12:47

Unit cell

4398 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)9.2650 +/- 0.0006
b (Angstrom)10.5290 +/- 0.0010
c (Angstrom)10.5971 +/- 0.0010
alpha (°)105.470 +/- 0.004
beta (°)99.119 +/- 0.005
gamma (°)93.955 +/- 0.005
Volume (A**3)976.97 +/- 0.15
Mosaicity (°)1.500 +/- 0.004

Data collection

Summary

Total number of images collected329
Total exposure time6.3 hours
Data collection exposure time6.3 hours
Data collection wall-clock time6.7 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°70 secondsYes
data collections02f17 34.0° omega2.000°70 secondsYes
data collections03f16 32.0° omega2.000°70 secondsYes
data collections04f25 50.0° omega2.000°70 secondsYes
data collections05f55110.0° omega2.000°70 secondsYes
data collections06f27 54.0° omega2.000°70 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 108
Zero sigma or profile test   4
Overload or incomplete profile 738
Sigma cutoff 128
High resolution limit 169

Final Data Set

Scale factor range9.86-11.94
Number of 'full' reflections  2561
Number of 'partial' reflections 19160
Total number of integrated reflections 20205
Total number of unique reflections  4455
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   22.7
Average Sigma(I)    1.7
Overall R-merge (linear)  0.085

Sadabs Results

Parameter refinement on 9346 reflections reduced R(int) from 0.0666 to 0.0524

Before rejection, 20021 reflections total and 4500 unique

After rejection, 19777 reflections total and 4500 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0867   0.914 - 1.062   0.924 - 1.419   1.230   11452    6045
    2   -8.7  0.0842   1.031 - 1.080   0.917 - 1.286   1.223     942     471
    3   -8.7  0.0835   0.976 - 1.033   0.980 - 1.166   1.194     868     455
    4   -8.7  0.0865   0.590 - 0.690   0.917 - 1.310   1.278    1457     788
    5   -8.7  0.0830   0.832 - 1.017   0.916 - 1.160   1.208    3464    1811
    6   -8.7  0.0810   0.510 - 0.568   0.917 - 1.260   1.201    1594     917
Ratio of minimum to maximum apparent transmission: 0.645780

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 a9  
  Formula   C8H15O4N1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.18 x 0.15 x 0.13 (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/