EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0806

Report generated Jul 02, 2007; 12:04:53

Unit cell

37147 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
a (Angstrom)11.9359 +/- 0.0003
b (Angstrom)17.2845 +/- 0.0005
c (Angstrom)21.4406 +/- 0.0006
alpha (°) 90.000
beta (°)92.5812 +/- 0.0017
gamma (°) 90.000
Volume (A**3)4418.8 +/- 0.2
Mosaicity (°)0.655 +/- 0.002

Data collection


Total number of images collected219
Total exposure time65.8 minutes
Data collection exposure time64.4 minutes
Data collection wall-clock time73.9 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance33.00 mm


TypeName# imagesTotal
Per frame
per frame
Used in
data collections01f151271.8° phi1.800°18 secondsYes
data collections02f60108.0° omega1.800°18 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   5
Zero sigma or profile test   1
Overload or incomplete profile1370
Sigma cutoff1270
Low resolution limit   7
High resolution limit  10

Final Data Set

Scale factor10.00
Number of 'full' reflections 24124
Number of 'partial' reflections 23892
Total number of integrated reflections 43441
Total number of unique reflections 10460
Data completeness  99.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   27.3
Average Sigma(I)    1.7
Overall R-merge (linear)  0.200

Sadabs Results

Parameter refinement on 26414 reflections reduced R(int) from 0.1725 to 0.0665

Before rejection, 46160 reflections total and 10522 unique

After rejection, 39822 reflections total and 10445 unique


  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   13.5  0.0931   0.729 - 1.227   0.986 - 1.152   2.093   28357   15810
    2   12.9  0.0944   0.579 - 0.871   0.990 - 1.122   2.044   11465    6257
Ratio of minimum to maximum apparent transmission: 0.855616


  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr Simon Aldridge  
  Local Code   AEJB 31  
  Formula   C29 H31 Fe1 B1 N1  
  Crystal Colour    Orange  
  Crystal Habit    Plate  
  Crystal Size   0.09 x 0.05 x 0.02 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

      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'

'COLLECT (Hooft, R.W.W., 1998)'
'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
'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/