EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/06skc0068

Report generated Nov 14, 2006; 14:03:36

Unit cell

2546 reflections with 0.41°<theta<28.28° (resolution between 50.00A and 0.75A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)8.339 +/- 0.002
b (Angstrom)11.266 +/- 0.003
c (Angstrom)11.902 +/- 0.002
alpha (°) 90.000
beta (°)98.327 +/- 0.016
gamma (°) 90.000
Volume (A**3)1106.5 +/- 0.4
Mosaicity (°)3.718 +/- 0.007

Data collection

Summary

Total number of images collected696
Total exposure time178.4 minutes
Data collection exposure time175.7 minutes
Data collection wall-clock time20.0 hours

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 collections01f363363.0° phi1.000°15 secondsYes
data collections02f27 27.0° omega1.000°15 secondsYes
data collections03f48 48.0° omega1.000°15 secondsYes
data collections04f49 49.0° omega1.000°15 secondsYes
data collections05f59 59.0° omega1.000°15 secondsYes
data collections06f49 49.0° omega1.000°15 secondsYes
data collections07f93 93.0° omega1.000°15 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 373
Zero sigma or profile test1078
Overload or incomplete profile1512
Sigma cutoff1937
High resolution limit 630

Final Data Set

Scale factor range2.63-10.65
Number of 'full' reflections     0
Number of 'partial' reflections 21360
Total number of integrated reflections 13536
Total number of unique reflections  2811
Data completeness  96.8%
Resolution range50.00-0.75 A
Theta range0.41°-28.28°
Average Intensity   15.5
Average Sigma(I)    2.0
Overall R-merge (linear)  0.200

Sadabs Results

Parameter refinement on 8382 reflections reduced R(int) from 0.1395 to 0.0755

Before rejection, 21897 reflections total and 5524 unique

After rejection, 19764 reflections total and 5487 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.1697   1.608 - 2.232   0.931 - 1.262   1.927   10576    4564
    2   11.1  0.2016   0.178 - 0.217   0.933 - 1.278   1.711     694     210
    3   11.1  0.1643   1.867 - 2.431   0.971 - 1.584   1.758    1356     423
    4   11.1  0.2496   1.419 - 1.908   0.931 - 1.559   1.650    1352     393
    5   11.1  0.2145   1.385 - 1.764   0.993 - 1.578   1.670    1716     528
    6   11.1  0.1894   1.820 - 2.590   0.931 - 1.533   1.743    1350     414
    7   11.1  0.2210   0.176 - 0.285   0.969 - 1.574   1.669    2720     884
Ratio of minimum to maximum apparent transmission: 0.587724

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp7 h1  
  Formula   C5H6O5N2  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.1 x 0.08 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 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/