EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0010

Report generated Feb 11, 2007; 20:03:19

Unit cell

2755 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)8.8551 +/- 0.0007
b (Angstrom)8.8489 +/- 0.0008
c (Angstrom)9.6793 +/- 0.0009
alpha (°)70.390 +/- 0.005
beta (°)70.366 +/- 0.005
gamma (°)77.328 +/- 0.006
Volume (A**3)668.04 +/- 0.10
Mosaicity (°)2.168 +/- 0.004

Data collection

Summary

Total number of images collected318
Total exposure time7.0 hours
Data collection exposure time6.9 hours
Data collection wall-clock time7.1 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°80 secondsYes
data collections02f13 26.0° omega2.000°80 secondsYes
data collections03f13 26.0° omega2.000°80 secondsYes
data collections04f53106.0° omega2.000°80 secondsYes
data collections05f25 50.0° omega2.000°80 secondsYes
data collections06f25 50.0° omega2.000°80 secondsYes
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Rejected 401
Zero sigma or profile test   2
Overload or incomplete profile 470
Sigma cutoff 260
High resolution limit  83

Final Data Set

Scale factor range7.40-10.47
Number of 'full' reflections     0
Number of 'partial' reflections 11731
Total number of integrated reflections  9993
Total number of unique reflections  3016
Data completeness  98.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  125.1
Average Sigma(I)    3.9
Overall R-merge (linear)  0.064

Sadabs Results

Parameter refinement on 9621 reflections reduced R(int) from 0.1140 to 0.0606

Before rejection, 11558 reflections total and 3095 unique

After rejection, 10419 reflections total and 3073 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.0507   1.019 - 1.634   0.939 - 1.270   1.986    6346    5364
    2   12.0  0.0672   0.295 - 0.314   0.975 - 1.276   2.227     356     315
    3   12.0  0.0612   0.587 - 0.625   0.979 - 1.198   2.174     355     310
    4   12.0  0.0769   0.575 - 0.689   0.939 - 1.540   2.150    1788    1513
    5   12.0  0.0710   0.485 - 0.593   0.978 - 1.471   2.150     794     630
    6   12.0  0.0761   0.555 - 0.654   0.983 - 1.390   2.172     780     642
Ratio of minimum to maximum apparent transmission: 0.609869

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp11 e5  
  Formula   C12H24O4N1  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.12 x 0.06 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 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    '10cm confocal mirrors'
_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/