EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/06skc0071

Report generated Nov 15, 2006; 13:12:23

Unit cell

4166 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)9.306 +/- 0.003
b (Angstrom)11.936 +/- 0.003
c (Angstrom)15.440 +/- 0.004
alpha (°)76.225 +/- 0.018
beta (°)74.830 +/- 0.014
gamma (°)89.749 +/- 0.017
Volume (A**3)1604.7 +/- 0.8
Mosaicity (°)4.681 +/- 0.010

Data collection

Summary

Total number of images collected351
Total exposure time129.0 minutes
Data collection exposure time127.6 minutes
Data collection wall-clock time143.4 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°22 secondsYes
data collections02f50100.0° omega2.000°22 secondsYes
data collections03f51102.0° omega2.000°22 secondsYes
data collections04f34 68.0° omega2.000°22 secondsYes
data collections05f48 96.0° omega2.000°22 secondsYes
data collections06f35 70.0° omega2.000°22 secondsYes
data collections07f51102.0° omega2.000°22 secondsYes
data collections08f23 46.0° omega2.000°22 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 676
Zero sigma or profile test 936
Overload or incomplete profile2512
Sigma cutoff2976
Low resolution limit  70
High resolution limit 121

Final Data Set

Scale factor range3.51-14.13
Number of 'full' reflections     0
Number of 'partial' reflections 27804
Total number of integrated reflections 15124
Total number of unique reflections  6123
Data completeness  78.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   10.5
Average Sigma(I)    2.1
Overall R-merge (linear)  0.224

Sadabs Results

Parameter refinement on 12394 reflections reduced R(int) from 0.2310 to 0.0993

Before rejection, 29992 reflections total and 7307 unique

After rejection, 24587 reflections total and 7226 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.6  0.2099   0.702 - 1.350   0.935 - 1.405   2.055    4159    1602
    2    5.7  0.4073   0.714 - 1.242   0.975 - 1.366   2.213    3535     726
    3   10.2  0.1918   0.548 - 0.870   0.941 - 1.319   1.991    4018    1603
    4   10.2  0.2237   0.660 - 0.879   0.942 - 1.610   2.094    2541     854
    5   10.2  0.1345   0.741 - 1.123   0.944 - 1.454   1.864    2806    1364
    6   10.2  0.1763   0.513 - 0.761   0.912 - 1.213   2.046    2491    1040
    7   10.2  0.1905   0.723 - 1.597   0.913 - 1.242   2.034    3794    1561
    8   10.2  0.5904   0.590 - 0.866   0.971 - 1.298   2.240    1243     207
Ratio of minimum to maximum apparent transmission: 0.566572

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp15 a4  
  Formula   C14H23O3N1S1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.19 x 0.13 x 0.03 (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    '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/