EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2008src0851

Report generated Jul 23, 2008; 16:43:31

Unit cell

19008 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p222
a (Angstrom)7.2251 +/- 0.0004
b (Angstrom)21.7492 +/- 0.0018
c (Angstrom)38.053 +/- 0.003
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)5979.6 +/- 0.8
Mosaicity (°)0.808 +/- 0.002

Data collection

Summary

Total number of images collected238
Total exposure time5.2 hours
Data collection exposure time5.1 hours
Data collection wall-clock time6.9 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance50.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f88176.0° phi2.000°80 secondsYes
data collections02f37 74.0° omega2.000°80 secondsYes
data collections03f68136.0° omega2.000°80 secondsYes
data collections04f37 74.0° omega2.000°80 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test 217
Overload or incomplete profile1132
Sigma cutoff 685
High resolution limit 113

Final Data Set

Scale factor10.00
Number of 'full' reflections 12280
Number of 'partial' reflections 13572
Total number of integrated reflections 19433
Total number of unique reflections  6229
Data completeness  81.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   27.8
Average Sigma(I)    2.3
Overall R-merge (linear)  0.136

Sadabs Results

Parameter refinement on 14608 reflections reduced R(int) from 0.1394 to 0.0648

Before rejection, 24359 reflections total and 6540 unique

After rejection, 20343 reflections total and 6404 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   24.7  0.0795   0.715 - 0.920   0.949 - 1.146   2.057    7399    4699
    2   23.5  0.1638   0.714 - 0.810   0.855 - 1.196   2.282    3406    1353
    3   17.0  0.0757   0.775 - 1.117   0.963 - 1.110   2.069    7081    4577
    4   24.1  0.0761   0.759 - 1.038   0.858 - 1.145   2.148    2457    1522
Ratio of minimum to maximum apparent transmission: 0.715221

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Dr A Kennedy  
  Local Code   FeH6AB1  
  Formula   C27H33N4O3Fe  
  Crystal Colour    Red  
  Crystal Habit    Needle  
  Crystal Size   0.2 x 0.01 x 0.01 (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/