EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2006src1371

Report generated Nov 22, 2006; 17:02:33

Unit cell

10873 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)13.6369 +/- 0.0005
b (Angstrom)15.0099 +/- 0.0005
c (Angstrom)15.0440 +/- 0.0006
alpha (°)89.686 +/- 0.002
beta (°)63.7940 +/- 0.0017
gamma (°)63.429 +/- 0.002
Volume (A**3)2399.19 +/- 0.17
Mosaicity (°)1.244 +/- 0.002

Data collection

Summary

Total number of images collected342
Total exposure time158.5 minutes
Data collection exposure time157.1 minutes
Data collection wall-clock time184.3 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f181362.0° phi2.000°28 secondsYes
data collections02f17 34.0° omega2.000°28 secondsYes
data collections03f56112.0° omega2.000°28 secondsYes
data collections04f56112.0° omega2.000°28 secondsYes
data collections05f24 48.0° omega2.000°28 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 316
Zero sigma or profile test   7
Overload or incomplete profile1962
Sigma cutoff 265
High resolution limit  51

Final Data Set

Scale factor range9.67-12.34
Number of 'full' reflections 12921
Number of 'partial' reflections 45046
Total number of integrated reflections 54854
Total number of unique reflections 11059
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   30.6
Average Sigma(I)    1.8
Overall R-merge (linear)  0.081

Sadabs Results

Parameter refinement on 30357 reflections reduced R(int) from 0.0974 to 0.0571

Before rejection, 54269 reflections total and 11084 unique

After rejection, 53583 reflections total and 11082 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0805   0.844 - 1.149   0.932 - 1.223   1.286   29378   17989
    2   -7.8  0.0808   0.625 - 0.654   0.960 - 1.244   1.241    2435    1464
    3   -7.8  0.0836   0.933 - 1.062   0.927 - 1.240   1.270    9098    5542
    4   -7.8  0.0824   0.726 - 0.824   0.945 - 1.204   1.280    9062    5532
    5   -7.8  0.0816   0.595 - 0.642   0.927 - 1.193   1.323    3610    2207
Ratio of minimum to maximum apparent transmission: 0.745128

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. A. Kennedy  
  Local Code   NiFeH6AE1  
  Formula   C54 H66 N8 S3 Ni2 Fe1  
  Crystal Colour    Light Violet  
  Crystal Habit    Rhombus  
  Crystal Size   0.3 x 0.24 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    'graphite'
_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/