EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0459

Report generated Apr 27, 2009; 10:32:01

Unit cell

9562 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)5.4433 +/- 0.0002
b (Angstrom)6.1440 +/- 0.0003
c (Angstrom)15.5205 +/- 0.0007
alpha (°)87.696 +/- 0.003
beta (°)84.420 +/- 0.003
gamma (°)70.454 +/- 0.002
Volume (A**3)486.82 +/- 0.04
Mosaicity (°)0.702 +/- 0.003

Data collection

Summary

Total number of images collected339
Total exposure time69.1 minutes
Data collection exposure time68.0 minutes
Data collection wall-clock time82.6 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 collections01f50100.0° omega2.000°12 secondsYes
data collections02f48 96.0° omega2.000°12 secondsYes
data collections03f50100.0° omega2.000°12 secondsYes
data collections04f48 96.0° omega2.000°12 secondsYes
data collections05f34 68.0° omega2.000°12 secondsYes
data collections06f51102.0° omega2.000°12 secondsYes
data collections07f50100.0° omega2.000°12 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected   3
Zero sigma or profile test   1
Overload or incomplete profile 344
Sigma cutoff 112
High resolution limit  23

Final Data Set

Scale factor10.00
Number of 'full' reflections  5533
Number of 'partial' reflections  5313
Total number of integrated reflections 10186
Total number of unique reflections  2218
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   78.4
Average Sigma(I)    2.0
Overall R-merge (linear)  0.142

Sadabs Results

Parameter refinement on 7864 reflections reduced R(int) from 0.1330 to 0.0582

Before rejection, 10006 reflections total and 2229 unique

After rejection, 8875 reflections total and 2218 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.1  0.0542   0.478 - 0.576   0.939 - 1.067   2.014    1395    1106
    2   10.8  0.0561   1.127 - 1.471   0.981 - 1.068   2.037    1269    1008
    3   10.2  0.0577   1.022 - 1.844   0.959 - 1.068   2.090    1301    1009
    4   10.2  0.0574   0.674 - 0.728   0.938 - 1.066   2.057    1315    1025
    5   10.2  0.0670   0.924 - 1.477   0.966 - 1.069   2.233     879     628
    6   10.2  0.0598   0.723 - 0.873   0.928 - 1.067   2.084    1361    1051
    7   10.2  0.0571   0.706 - 1.055   0.955 - 1.069   2.030    1355    1048
Ratio of minimum to maximum apparent transmission: 0.867714

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   HP160  
  Formula   C10H13N3O  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.09 x 0.06 x 0.04 (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/