EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0288r

Report generated Mar 11, 2009; 08:32:45

Unit cell

21695 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)7.7714 +/- 0.0006
b (Angstrom)10.0042 +/- 0.0007
c (Angstrom)10.1601 +/- 0.0007
alpha (°)112.144 +/- 0.004
beta (°)103.536 +/- 0.003
gamma (°)107.454 +/- 0.003
Volume (A**3)641.85 +/- 0.09
Mosaicity (°)1.404 +/- 0.003

Data collection

Summary

Total number of images collected389
Total exposure time11.7 hours
Data collection exposure time11.7 hours
Data collection wall-clock time12.3 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°110 secondsYes
data collections02f13 26.0° omega2.000°110 secondsYes
data collections03f27 54.0° omega2.000°110 secondsYes
data collections04f52104.0° omega2.000°110 secondsYes
data collections05f53106.0° omega2.000°110 secondsYes
data collections06f55110.0° omega2.000°110 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Zero sigma or profile test   1
Overload or incomplete profile 418
Sigma cutoff 248
Low resolution limit  19
High resolution limit  15

Final Data Set

Scale factor10.00
Number of 'full' reflections  2166
Number of 'partial' reflections 11128
Total number of integrated reflections 11621
Total number of unique reflections  2962
Data completeness  97.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   90.3
Average Sigma(I)    3.3
Overall R-merge (linear)  0.124

Sadabs Results

Parameter refinement on 9373 reflections reduced R(int) from 0.0974 to 0.0653

Before rejection, 12491 reflections total and 2989 unique

After rejection, 11095 reflections total and 2973 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0657   0.899 - 1.109   0.933 - 1.097   2.053    5325    3979
    2   14.6  0.0629   0.458 - 0.521   0.976 - 1.095   2.102     305     215
    3   14.6  0.0773   0.527 - 0.627   0.994 - 1.117   2.320     745     526
    4   14.6  0.0593   0.862 - 1.053   0.974 - 1.137   2.071    1559    1192
    5   14.6  0.0589   0.805 - 0.993   0.957 - 1.120   2.015    1557    1204
    6   14.6  0.0665   0.763 - 0.916   0.933 - 1.116   2.108    1604    1221
Ratio of minimum to maximum apparent transmission: 0.820601

Metadata

  Group    Service  
  Operator   Richard Stephenson  
  Sample Owner   Prof Peter Taylor  
  Local Code   C9H12Cl2N2O3Si1  
  Formula     
  Crystal Colour    Brown  
  Crystal Habit    Fragment  
  Crystal Size   0.12 x 0.05 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/