EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0461r

Report generated Apr 29, 2009; 16:46:48

Unit cell

15253 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)6.1693 +/- 0.0005
b (Angstrom)7.0845 +/- 0.0006
c (Angstrom)10.3537 +/- 0.0008
alpha (°)87.871 +/- 0.005
beta (°)74.394 +/- 0.005
gamma (°)69.471 +/- 0.005
Volume (A**3)407.34 +/- 0.06
Mosaicity (°)1.571 +/- 0.005

Data collection

Summary

Total number of images collected321
Total exposure time128.9 minutes
Data collection exposure time126.9 minutes
Data collection wall-clock time145.5 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°24 secondsYes
data collections02f51102.0° omega2.000°24 secondsYes
data collections03f45 90.0° omega2.000°24 secondsYes
data collections04f48 96.0° omega2.000°24 secondsYes
data collections05f23 46.0° omega2.000°24 secondsYes
data collections06f45 90.0° omega2.000°24 secondsYes
data collections07f50100.0° omega2.000°24 secondsYes
Phi/Chii01f - i08f815 seconds

Scalepack Scaling

Deleted observations

Overload or incomplete profile 318
Sigma cutoff 186
High resolution limit 264

Final Data Set

Scale factor10.00
Number of 'full' reflections   738
Number of 'partial' reflections  7767
Total number of integrated reflections  7376
Total number of unique reflections  1795
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   80.4
Average Sigma(I)    2.6
Overall R-merge (linear)  0.230

Sadabs Results

Parameter refinement on 5738 reflections reduced R(int) from 0.1926 to 0.0701

Before rejection, 7868 reflections total and 1872 unique

After rejection, 6884 reflections total and 1862 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0504   0.665 - 0.851   0.916 - 1.419   2.006    1140     862
    2    7.2  0.0547   0.681 - 1.229   0.952 - 1.095   2.095    1161     862
    3   10.2  0.0506   0.816 - 1.065   0.958 - 1.123   2.010    1013     778
    4   10.2  0.0775   0.779 - 1.298   0.970 - 1.094   2.254    1072     682
    5   10.2  0.1064   0.836 - 1.187   0.966 - 1.457   2.465     437     229
    6   10.2  0.0542   0.288 - 0.503   0.964 - 1.079   2.076    1003     751
    7   10.2  0.0638   1.587 - 2.935   0.899 - 1.096   2.123    1058     741
Ratio of minimum to maximum apparent transmission: 0.616905

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J. Spencer  
  Local Code   HP155  
  Formula   C8H5N3OS  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.11 x 0.06 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/