EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007jmw0007

Report generated Feb 27, 2007; 18:29:51

Unit cell

2748 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)7.8166 +/- 0.0003
b (Angstrom)9.2417 +/- 0.0002
c (Angstrom)10.0603 +/- 0.0003
alpha (°)85.445 +/- 0.002
beta (°)67.9680 +/- 0.0018
gamma (°)79.532 +/- 0.002
Volume (A**3)662.41 +/- 0.04
Mosaicity (°)0.487 +/- 0.002

Data collection

Summary

Total number of images collected284
Total exposure time233.5 minutes
Data collection exposure time231.4 minutes
Data collection wall-clock time248.4 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f51102.0° omega2.000°50 secondsYes
data collections02f51102.0° omega2.000°50 secondsYes
data collections03f51102.0° omega2.000°50 secondsYes
data collections04f42 84.0° omega2.000°50 secondsYes
data collections05f48 96.0° omega2.000°50 secondsYes
data collections06f33 66.0° omega2.000°50 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Rejected 693
Overload or incomplete profile 364
Sigma cutoff  89
High resolution limit  95

Final Data Set

Scale factor range9.16-27.15
Number of 'full' reflections  7461
Number of 'partial' reflections  4160
Total number of integrated reflections 11065
Total number of unique reflections  2970
Data completeness  99.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   67.1
Average Sigma(I)    1.8
Overall R-merge (linear)  0.068

Sadabs Results

Parameter refinement on 9488 reflections reduced R(int) from 0.1625 to 0.0632

Before rejection, 11489 reflections total and 3035 unique

After rejection, 10247 reflections total and 3021 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.5  0.0745   0.890 - 1.236   0.974 - 1.099   2.244    1936    1495
    2   10.2  0.0510   0.645 - 1.347   0.957 - 1.100   1.968    1859    1610
    3   10.2  0.0572   0.676 - 1.402   0.987 - 1.093   2.079    1925    1600
    4   10.2  0.0384   0.587 - 0.721   0.941 - 1.060   1.738    1574    1436
    5   10.2  0.0600   0.699 - 0.946   0.947 - 1.071   2.133    1760    1451
    6   10.2  0.0593   0.641 - 0.802   0.947 - 1.086   2.096    1193    1001
Ratio of minimum to maximum apparent transmission: 0.855434

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CC 47839  
  Formula   C12 H17 B1 O4 S1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Plate  
  Crystal Size   0.16 x 0.08 x 0.02 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent   Hexane  
  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    '10cm confocal mirrors'
_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/