EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src1136

Report generated Nov 26, 2009; 13:14:08

Unit cell

51227 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)8.8505 +/- 0.0002
b (Angstrom)16.2148 +/- 0.0005
c (Angstrom)16.5501 +/- 0.0004
alpha (°)96.9675 +/- 0.0012
beta (°)93.6643 +/- 0.0017
gamma (°)90.3070 +/- 0.0016
Volume (A**3)2352.52 +/- 0.11
Mosaicity (°)0.7350 +/- 0.0010

Data collection

Summary

Total number of images collected475
Total exposure time190.7 minutes
Data collection exposure time189.3 minutes
Data collection wall-clock time213.1 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f242363.0° phi1.500°24 secondsYes
data collections02f17 25.5° omega1.500°24 secondsYes
data collections03f18 27.0° omega1.500°24 secondsYes
data collections04f36 54.0° omega1.500°24 secondsYes
data collections05f74111.0° omega1.500°24 secondsYes
data collections06f27 40.5° omega1.500°24 secondsYes
data collections07f26 39.0° omega1.500°24 secondsYes
data collections08f27 40.5° omega1.500°24 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   8
Zero sigma or profile test  19
Overload or incomplete profile1402
Sigma cutoff 760
High resolution limit 102

Final Data Set

Scale factor10.00
Number of 'full' reflections 16168
Number of 'partial' reflections 28690
Total number of integrated reflections 41232
Total number of unique reflections 10738
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   48.0
Average Sigma(I)    1.9
Overall R-merge (linear)  0.138

Sadabs Results

Parameter refinement on 29450 reflections reduced R(int) from 0.1036 to 0.0605

Before rejection, 41736 reflections total and 10793 unique

After rejection, 36398 reflections total and 10724 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0669   0.775 - 1.082   0.985 - 1.138   2.039   19308   13502
    2   14.6  0.0783   0.742 - 0.813   0.995 - 1.136   2.142    1170     749
    3   14.6  0.0847   0.695 - 0.736   0.993 - 1.141   2.129    1264     774
    4   14.6  0.0616   0.831 - 0.945   0.995 - 1.130   2.038    2790    2025
    5   14.6  0.0669   0.691 - 0.915   0.988 - 1.095   1.975    5874    4107
    6   14.6  0.0629   0.797 - 0.931   0.985 - 1.065   1.975    2045    1474
    7   14.6  0.0668   0.803 - 0.904   0.995 - 1.096   2.034    1928    1352
    8   14.6  0.0627   0.668 - 0.783   0.984 - 1.126   1.927    2019    1439
Ratio of minimum to maximum apparent transmission: 0.862603

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr L Martin  
  Local Code   LeeMnFeOx3  
  Formula   C37 H26 O12 S24 Cl2 Fe Mn  
  Crystal Colour    Dark Orange  
  Crystal Habit    Sheet  
  Crystal Size   0.1 x 0.08 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/