EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src1061

Report generated Sep 05, 2005; 15:24:31

Unit cell

3467 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)6.71030 +/- 0.00010
b (Angstrom)9.9712 +/- 0.0003
c (Angstrom)12.0253 +/- 0.0004
alpha (°)106.0923 +/- 0.0014
beta (°)90.9138 +/- 0.0018
gamma (°)90.8274 +/- 0.0018
Volume (A**3)772.83 +/- 0.04
Mosaicity (°)0.806 +/- 0.002

Data collection

Summary

Total number of images collected350
Total exposure time58.9 minutes
Data collection exposure time58.2 minutes
Data collection wall-clock time86.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°10 secondsYes
data collections02f16 32.0° omega2.000°10 secondsYes
data collections03f16 32.0° omega2.000°10 secondsYes
data collections04f22 44.0° omega2.000°10 secondsYes
data collections05f54108.0° omega2.000°10 secondsYes
data collections06f53106.0° omega2.000°10 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 109
Overload or incomplete profile 858
Sigma cutoff  14
High resolution limit  18

Final Data Set

Scale factor range5.56-11.71
Number of 'full' reflections  8865
Number of 'partial' reflections 11033
Total number of integrated reflections 18866
Total number of unique reflections  3533
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  287.1
Average Sigma(I)    6.0
Overall R-merge (linear)  0.040

Sadabs Results

Parameter refinement on 16452 reflections reduced R(int) from 0.0963 to 0.0343

Before rejection, 18543 reflections total and 3544 unique

After rejection, 18318 reflections total and 3543 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0312   0.841 - 1.039   0.917 - 1.216   1.386    9746    8939
    2   -6.1  0.0396   0.772 - 0.835   0.935 - 1.168   1.506     793     692
    3   -6.8  0.0395   0.862 - 1.086   0.917 - 1.174   1.504     774     671
    4   -6.8  0.0575   0.830 - 0.920   0.917 - 1.179   1.537    1141     983
    5   -6.8  0.0345   0.834 - 1.890   0.930 - 1.179   1.414    2971    2684
    6   -6.8  0.0358   0.703 - 1.201   0.930 - 1.175   1.401    2893    2596
Ratio of minimum to maximum apparent transmission: 0.754113

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Aldridge  
  Local Code   NDC57  
  Formula   C25H34FeBrInO2  
  Crystal Colour    Orange  
  Crystal Habit    Plate  
  Crystal Size   0.1 x 0.1 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/