EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)


Summary report for Directory: diska/2009src0113

Report generated Feb 11, 2009; 12:22:55

Unit cell

25207 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack
p2
a (Angstrom)15.8650 +/- 0.0012
b (Angstrom)5.6205 +/- 0.0004
c (Angstrom)16.4742 +/- 0.0012
alpha (°) 90.000
beta (°)106.779 +/- 0.004
gamma (°) 90.000
Volume (A**3)1406.45 +/- 0.18
Mosaicity (°)1.197 +/- 0.004

Data collection

Summary

Total number of images collected227
Total exposure time114.0 minutes
Data collection exposure time110.7 minutes
Data collection wall-clock time120.5 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°30 secondsYes
data collections02f48 96.0° omega2.000°30 secondsYes
data collections03f47 94.0° omega2.000°30 secondsYes
data collections04f44 88.0° omega2.000°30 secondsYes
data collections05f29 58.0° omega2.000°30 secondsYes
Phi/Chii01f - i08f825 seconds

Scalepack Scaling

Deleted observations

Rejected   3
Zero sigma or profile test   8
Overload or incomplete profile 872
Sigma cutoff 632
High resolution limit  93

Final Data Set

Scale factor10.00
Number of 'full' reflections  5030
Number of 'partial' reflections 16180
Total number of integrated reflections 18568
Total number of unique reflections  3516
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   12.3
Average Sigma(I)    1.0
Overall R-merge (linear)  0.257

Sadabs Results

Parameter refinement on 9735 reflections reduced R(int) from 0.1641 to 0.0828

Before rejection, 19193 reflections total and 3567 unique

After rejection, 16409 reflections total and 3556 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.2  0.1233   0.591 - 1.143   0.974 - 1.552   1.981    3864    1908
    2   10.2  0.1334   0.635 - 1.031   0.975 - 1.187   2.017    3595    1651
    3   10.2  0.1344   0.750 - 1.094   0.974 - 1.347   2.056    3552    1681
    4    6.5  0.1324   0.684 - 0.987   1.003 - 1.355   2.062    3406    1516
    5   10.2  0.1619   0.646 - 0.819   0.989 - 1.379   2.046    1992     853
Ratio of minimum to maximum apparent transmission: 0.627880

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr J Spencer  
  Local Code   HP153(C)AMINO  
  Formula   C16H17FN4O  
  Crystal Colour    Colourless  
  Crystal Habit    Lath  
  Crystal Size   0.43 x 0.05 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/