EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2006src1117

Report generated Nov 01, 2006; 09:23:41

Unit cell

4377 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)8.1247 +/- 0.0002
b (Angstrom)17.1558 +/- 0.0004
c (Angstrom)13.9097 +/- 0.0003
alpha (°) 90.000
beta (°)105.9609 +/- 0.0014
gamma (°) 90.000
Volume (A**3)1864.07 +/- 0.08
Mosaicity (°)0.4750 +/- 0.0010

Data collection

Summary

Total number of images collected330
Total exposure time12.2 hours
Data collection exposure time12.1 hours
Data collection wall-clock time12.5 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance40.00 mm

Scans

TypeName# imagesTotal
Rotation
Per frame
Rotation
Exposure
per frame
Used in
scaling
data collections01f152228.0° phi1.500°135 secondsYes
data collections02f87130.5° omega1.500°135 secondsYes
data collections03f83124.5° omega1.500°135 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected 217
Overload or incomplete profile 440
Sigma cutoff  34
High resolution limit   7

Final Data Set

Scale factor range7.00-10.99
Number of 'full' reflections 13054
Number of 'partial' reflections  9805
Total number of integrated reflections 22222
Total number of unique reflections  4428
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   86.0
Average Sigma(I)    3.1
Overall R-merge (linear)  0.070

Sadabs Results

Parameter refinement on 15900 reflections reduced R(int) from 0.1806 to 0.0485

Before rejection, 22297 reflections total and 4434 unique

After rejection, 21950 reflections total and 4434 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.6  0.0544   0.983 - 1.533   0.831 - 1.755   1.397   10128    7627
    2  -15.0  0.0644   0.967 - 1.879   0.846 - 1.710   1.368    6066    4383
    3  -15.0  0.0520   0.470 - 0.572   0.831 - 1.362   1.270    5756    4454
Ratio of minimum to maximum apparent transmission: 0.473539

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr. A. Kennedy  
  Local Code   ZnAE1  
  Formula   C36 H54 N4 S4 Br2 Zn1  
  Crystal Colour    Colourless  
  Crystal Habit    Shard  
  Crystal Size   0.24 x 0.07 x 0.05 (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/