EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: home/diska/06skc0016

Report generated Jun 05, 2006; 09:03:36

Unit cell

3727 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)6.1325 +/- 0.0004
b (Angstrom)10.2549 +/- 0.0007
c (Angstrom)13.7449 +/- 0.0006
alpha (°)98.276 +/- 0.003
beta (°)93.844 +/- 0.004
gamma (°)94.426 +/- 0.003
Volume (A**3)850.16 +/- 0.09
Mosaicity (°)0.858 +/- 0.003

Data collection

Summary

Total number of images collected293
Total exposure time97.4 minutes
Data collection exposure time96.0 minutes
Data collection wall-clock time133.2 minutes

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°20 secondsYes
data collections02f16 32.0° omega2.000°20 secondsYes
data collections03f16 32.0° omega2.000°20 secondsYes
data collections04f56112.0° omega2.000°20 secondsYes
data collections05f16 32.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 125
Zero sigma or profile test   4
Overload or incomplete profile 708
Sigma cutoff  13
High resolution limit   1

Final Data Set

Scale factor range5.97-15.37
Number of 'full' reflections  6926
Number of 'partial' reflections  9681
Total number of integrated reflections 15719
Total number of unique reflections  3892
Data completeness  98.5%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   30.0
Average Sigma(I)    1.7
Overall R-merge (linear)  0.094

Sadabs Results

Parameter refinement on 9664 reflections reduced R(int) from 0.1749 to 0.0614

Before rejection, 15406 reflections total and 3899 unique

After rejection, 15078 reflections total and 3899 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0790   0.841 - 1.781   0.933 - 1.219   1.407    9807    6610
    2   -8.7  0.0675   0.321 - 0.380   0.929 - 1.211   1.402     772     566
    3   -8.7  0.0632   0.480 - 0.539   0.941 - 1.052   1.293     758     533
    4   -8.7  0.0709   0.570 - 0.865   0.929 - 1.179   1.347    3059    2201
    5   -8.7  0.1254   0.579 - 0.626   0.929 - 1.209   1.462     682     347
Ratio of minimum to maximum apparent transmission: 0.761943

Metadata

  Group    Service  
  Operator     
  Sample Owner     
  Local Code     
  Formula     
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.2 x 0.2 x 0.2 (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/