EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/06skc0082

Report generated Feb 05, 2007; 16:45:40

Unit cell

4421 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)7.0534 +/- 0.0003
b (Angstrom)7.5192 +/- 0.0003
c (Angstrom)18.9308 +/- 0.0008
alpha (°)79.448 +/- 0.002
beta (°)90.040 +/- 0.003
gamma (°)89.992 +/- 0.002
Volume (A**3)987.03 +/- 0.07
Mosaicity (°)1.282 +/- 0.002

Data collection

Summary

Total number of images collected1342
Total exposure time230.8 minutes
Data collection exposure time229.4 minutes
Data collection wall-clock time295.5 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance36.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f363363.0° phi1.000°10 secondsYes
data collections02f27 27.0° omega1.000°10 secondsYes
data collections03f29 29.0° omega1.000°10 secondsYes
data collections04f113113.0° omega1.000°10 secondsYes
data collections05f57 57.0° omega1.000°10 secondsYes
data collections06f62 62.0° omega1.000°10 secondsYes
data collections07f113113.0° omega1.000°10 secondsYes
data collections08f113113.0° omega1.000°10 secondsYes
data collections09f111111.0° omega1.000°10 secondsYes
data collections10f78 78.0° omega1.000°10 secondsNo
data collections11f113113.0° omega1.000°10 secondsNo
data collections12f97 97.0° omega1.000°10 secondsNo
data collections13f58 58.0° omega1.000°10 secondsNo
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 519
Zero sigma or profile test  37
Overload or incomplete profile 804
Sigma cutoff 481
High resolution limit 145

Final Data Set

Scale factor range3.61-13.32
Number of 'full' reflections     0
Number of 'partial' reflections 24407
Total number of integrated reflections 21259
Total number of unique reflections  4523
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   37.8
Average Sigma(I)    1.4
Overall R-merge (linear)  0.079

Sadabs Results

Parameter refinement on 23632 reflections reduced R(int) from 0.1109 to 0.0554

Before rejection, 32959 reflections total and 4571 unique

After rejection, 28732 reflections total and 4569 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.0584   0.769 - 1.085   0.979 - 1.153   2.023    7852    5491
    2   15.4  0.0513   0.753 - 0.865   1.003 - 1.095   2.024     521     382
    3   12.4  0.1326   0.495 - 0.609   0.985 - 1.142   2.208     599     304
    4   15.4  0.0726   0.782 - 1.369   0.980 - 1.195   2.120    2463    1494
    5   15.4  0.0933   0.663 - 0.844   0.994 - 1.100   2.153    1192     680
    6   15.4  0.0573   0.725 - 0.807   0.979 - 1.180   1.937    1325     969
    7   15.4  0.0827   0.811 - 1.575   0.978 - 1.153   2.122    2450    1533
    8   15.4  0.0588   0.716 - 1.076   0.981 - 1.167   2.044    2481    1702
    9   15.4  0.0541   0.756 - 1.068   0.979 - 1.130   1.928    2407    1794
   10   15.4  0.0535   0.701 - 0.865   0.992 - 1.176   1.955    1670    1210
   11   15.4  0.0506   0.788 - 0.995   0.989 - 1.131   2.000    2476    1846
   12   15.4  0.0546   0.757 - 0.883   0.979 - 1.073   1.993    2067    1439
   13   15.4  0.0542   0.697 - 0.818   1.000 - 1.144   1.951    1229     889
Ratio of minimum to maximum apparent transmission: 0.818688

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp16 b6  
  Formula   C8H612O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.1 x 0.08 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 V2.10 (Sheldrick, G.M., 2003)'

_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 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   9.091

_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. (2003). SADABS. Version 2.10. 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/