EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007may0016

Report generated Jul 12, 2007; 11:34:38

Unit cell

55607 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)10.0846 +/- 0.0003
b (Angstrom)10.4718 +/- 0.0003
c (Angstrom)10.9149 +/- 0.0003
alpha (°)106.7179 +/- 0.0014
beta (°)111.4728 +/- 0.0015
gamma (°)95.6034 +/- 0.0015
Volume (A**3)1000.33 +/- 0.05
Mosaicity (°)1.0740 +/- 0.0010

Data collection

Summary

Total number of images collected733
Total exposure time10.2 hours
Data collection exposure time10.1 hours
Data collection wall-clock time10.7 hours

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 collections01f102102.0° omega1.000°50 secondsYes
data collections02f98 98.0° omega1.000°50 secondsYes
data collections03f48 48.0° omega1.000°50 secondsYes
data collections04f102102.0° omega1.000°50 secondsYes
data collections05f76 76.0° omega1.000°50 secondsYes
data collections06f96 96.0° omega1.000°50 secondsYes
data collections07f67 67.0° omega1.000°50 secondsYes
data collections08f47 47.0° omega1.000°50 secondsYes
data collections09f89 89.0° omega1.000°50 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected   7
Zero sigma or profile test   1
Overload or incomplete profile1142
Sigma cutoff 688
High resolution limit  10

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 24146
Total number of integrated reflections 21116
Total number of unique reflections  4593
Data completeness  99.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  210.4
Average Sigma(I)    5.5
Overall R-merge (linear)  0.129

Sadabs Results

Parameter refinement on 17443 reflections reduced R(int) from 0.1283 to 0.0742

Before rejection, 22739 reflections total and 4616 unique

After rejection, 20443 reflections total and 4593 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.2  0.0822   0.928 - 1.399   0.914 - 1.106   2.118    2941    2225
    2   10.0  0.0680   1.059 - 1.396   0.944 - 1.116   2.116    2832    2129
    3   10.2  0.0812   0.505 - 0.577   0.911 - 1.101   1.984    1307     980
    4   10.2  0.0781   0.979 - 1.311   0.911 - 1.096   2.009    2886    2214
    5   10.2  0.0711   1.218 - 1.509   0.933 - 1.117   2.099    2113    1637
    6   10.2  0.0609   1.076 - 1.411   0.915 - 1.116   2.079    2725    2067
    7   10.2  0.0747   0.424 - 0.649   0.977 - 1.090   2.057    1871    1412
    8   10.2  0.0663   0.349 - 0.429   0.978 - 1.089   2.000    1255     951
    9   10.2  0.0628   0.655 - 0.806   0.913 - 1.114   2.050    2513    1956
Ratio of minimum to maximum apparent transmission: 0.815889

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CC 30617  
  Formula   C6 H7 N1 O1 S1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.06 x 0.06 x 0.02 (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/