EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/06skc0027

Report generated Sep 19, 2006; 17:54:21

Unit cell

2644 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)7.5274 +/- 0.0003
b (Angstrom)9.4023 +/- 0.0004
c (Angstrom)9.9905 +/- 0.0004
alpha (°)64.267 +/- 0.002
beta (°)68.175 +/- 0.002
gamma (°)74.172 +/- 0.002
Volume (A**3)586.04 +/- 0.04
Mosaicity (°)0.798 +/- 0.002

Data collection

Summary

Total number of images collected586
Total exposure time119.0 minutes
Data collection exposure time117.6 minutes
Data collection wall-clock time165.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f302362.4° phi1.200°12 secondsYes
data collections02f27 32.4° omega1.200°12 secondsYes
data collections03f27 32.4° omega1.200°12 secondsYes
data collections04f92110.4° omega1.200°12 secondsYes
data collections05f40 48.0° omega1.200°12 secondsYes
data collections06f90108.0° omega1.200°12 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 158
Zero sigma or profile test   4
Overload or incomplete profile 514
Sigma cutoff   4
High resolution limit  29

Final Data Set

Scale factor range6.77-11.96
Number of 'full' reflections  2806
Number of 'partial' reflections 11707
Total number of integrated reflections 13948
Total number of unique reflections  2679
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   36.3
Average Sigma(I)    1.5
Overall R-merge (linear)  0.073

Sadabs Results

Parameter refinement on 9135 reflections reduced R(int) from 0.0974 to 0.0550

Before rejection, 13944 reflections total and 2691 unique

After rejection, 13651 reflections total and 2691 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0638   0.934 - 1.196   0.961 - 1.136   1.413    7101    5023
    2   -7.8  0.0547   0.578 - 0.627   0.961 - 1.069   1.445     602     426
    3   -7.8  0.0801   0.620 - 0.706   0.961 - 1.134   1.409     608     392
    4   -7.8  0.0749   0.627 - 0.737   0.960 - 1.056   1.436    2236    1442
    5   -7.8  0.0727   0.663 - 0.906   0.961 - 1.127   1.491     923     578
    6   -7.8  0.0674   0.711 - 1.177   0.961 - 1.083   1.447    2181    1435
Ratio of minimum to maximum apparent transmission: 0.845338

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 e10  
  Formula   C9H14O6N2  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.08 x 0.07 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/