EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0949

Report generated Sep 01, 2009; 13:42:24

Unit cell

10941 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)7.2314 +/- 0.0002
b (Angstrom)9.4760 +/- 0.0003
c (Angstrom)11.6165 +/- 0.0004
alpha (°)82.0938 +/- 0.0016
beta (°)82.082 +/- 0.002
gamma (°)78.631 +/- 0.002
Volume (A**3)767.95 +/- 0.04
Mosaicity (°)0.544 +/- 0.002

Data collection

Summary

Total number of images collected346
Total exposure time81.8 minutes
Data collection exposure time80.7 minutes
Data collection wall-clock time100.1 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°14 secondsYes
data collections02f13 26.0° omega2.000°14 secondsYes
data collections03f13 26.0° omega2.000°14 secondsYes
data collections04f53106.0° omega2.000°14 secondsYes
data collections05f25 50.0° omega2.000°14 secondsYes
data collections06f26 52.0° omega2.000°14 secondsYes
data collections07f27 54.0° omega2.000°14 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test   1
Overload or incomplete profile 520
Sigma cutoff 107
High resolution limit  24

Final Data Set

Scale factor10.00
Number of 'full' reflections  9601
Number of 'partial' reflections  6134
Total number of integrated reflections 14894
Total number of unique reflections  3524
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  126.7
Average Sigma(I)    2.9
Overall R-merge (linear)  0.109

Sadabs Results

Parameter refinement on 12199 reflections reduced R(int) from 0.0715 to 0.0437

Before rejection, 14673 reflections total and 3536 unique

After rejection, 13300 reflections total and 3527 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   12.6  0.0459   0.839 - 1.092   0.989 - 1.064   2.173    7321    6126
    2   12.0  0.0436   0.266 - 0.295   0.994 - 1.054   2.124     454     371
    3   12.0  0.0416   0.797 - 0.866   0.990 - 1.041   1.951     441     366
    4   12.0  0.0373   1.232 - 1.576   0.989 - 1.053   2.093    2124    1747
    5   12.0  0.0410   0.765 - 0.900   0.994 - 1.043   2.092     927     729
    6   12.0  0.0516   0.761 - 0.939   0.989 - 1.030   2.107     988     792
    7   12.0  0.0377   0.825 - 0.964   0.993 - 1.055   2.001    1045     877
Ratio of minimum to maximum apparent transmission: 0.929910

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr PJ Holliman  
  Local Code   ACHFSQ3  
  Formula   C18 H19 O3 N  
  Crystal Colour    Orange  
  Crystal Habit    Slab  
  Crystal Size   0.16 x 0.11 x 0.05 (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/