EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/07skc0022

Report generated Feb 19, 2007; 08:18:36

Unit cell

4271 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)7.6467 +/- 0.0008
b (Angstrom)11.2028 +/- 0.0011
c (Angstrom)11.6723 +/- 0.0009
alpha (°)90.011 +/- 0.006
beta (°)90.029 +/- 0.006
gamma (°)86.450 +/- 0.005
Volume (A**3)997.98 +/- 0.16
Mosaicity (°)1.738 +/- 0.004

Data collection

Summary

Total number of images collected391
Total exposure time12.9 hours
Data collection exposure time12.8 hours
Data collection wall-clock time13.1 hours

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 collections01f181362.0° phi2.000°120 secondsYes
data collections02f15 30.0° omega2.000°120 secondsYes
data collections03f13 26.0° omega2.000°120 secondsYes
data collections04f56112.0° omega2.000°120 secondsYes
data collections05f28 56.0° omega2.000°120 secondsYes
data collections06f34 68.0° omega2.000°120 secondsYes
data collections07f56112.0° omega2.000°120 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected 615
Overload or incomplete profile 708
Sigma cutoff 861
High resolution limit 243

Final Data Set

Scale factor range7.22-14.22
Number of 'full' reflections   868
Number of 'partial' reflections 18779
Total number of integrated reflections 16594
Total number of unique reflections  4505
Data completeness  99.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   27.1
Average Sigma(I)    1.9
Overall R-merge (linear)  0.134

Sadabs Results

Parameter refinement on 9976 reflections reduced R(int) from 0.2510 to 0.0780

Before rejection, 18589 reflections total and 4620 unique

After rejection, 15730 reflections total and 4587 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.1172   2.150 - 5.805   0.971 - 1.273   2.071    7710    3879
    2   10.5  0.0891   0.151 - 0.165   1.023 - 1.305   1.987     520     311
    3   15.4  0.1051   0.168 - 0.180   0.981 - 1.246   2.195     446     235
    4   15.4  0.0971   2.020 - 2.454   0.983 - 1.136   1.987    2302    1236
    5   15.4  0.1049   0.160 - 0.177   0.979 - 1.193   2.101    1115     590
    6   15.4  0.0981   0.429 - 0.496   0.971 - 1.138   2.000    1342     731
    7   15.4  0.1030   1.825 - 2.281   0.993 - 1.251   2.031    2295    1254
Ratio of minimum to maximum apparent transmission: 0.743658

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp13 e8  
  Formula   C9H12O4N2  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.08 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 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/