EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/06skc0012

Report generated Mar 19, 2006; 08:52:20

Unit cell

2566 reflections with 1.00°<theta<23.26° (resolution between 20.40A and 0.90A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)8.1971 +/- 0.0010
b (Angstrom)14.6660 +/- 0.0015
c (Angstrom)14.340 +/- 0.002
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)1723.9 +/- 0.4
Mosaicity (°)2.138 +/- 0.004

Data collection

Summary

Total number of images collected686
Total exposure time5.2 hours
Data collection exposure time5.1 hours
Data collection wall-clock time7.8 hours

Experimental Conditions

Wavelength0.71073 A

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Detector
distance		Used in
scaling
cell determinationi01f10 10.0° phi1.000°20 seconds45.00 mmNo
data collections01f213191.7° phi0.900°27 seconds34.00 mmYes
data collections02f60 54.0° omega0.900°27 seconds34.00 mmYes
data collections03f76 68.4° omega0.900°27 seconds34.00 mmYes
data collections04f116104.4° omega0.900°27 seconds34.00 mmYes
data collections05f85 76.5° omega0.900°27 seconds34.00 mmYes
data collections06f126113.4° omega0.900°27 seconds34.00 mmYes

Scalepack Scaling

Deleted observations

Rejected 114
Zero sigma or profile test 155
Overload or incomplete profile1512
Sigma cutoff 164
High resolution limit 264

Final Data Set

Scale factor range9.96-10.70
Number of 'full' reflections     0
Number of 'partial' reflections 23144
Total number of integrated reflections 18762
Total number of unique reflections  2586
Data completeness  99.7%
Resolution range20.40-0.90 A
Theta range1.00°-23.26°
Average Intensity   12.5
Average Sigma(I)    1.2
Overall R-merge (linear)  0.129

Sadabs Results

Parameter refinement on 9839 reflections reduced R(int) from 0.0811 to 0.0659

Before rejection, 23472 reflections total and 1479 unique

After rejection, 23268 reflections total and 1476 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.0  0.1671   1.094 - 1.555   0.876 - 1.196   1.190    7194    3389
    2  -10.4  0.1439   0.495 - 0.552   0.942 - 1.070   1.128    2019    1085
    3  -10.4  0.2254   0.709 - 0.903   0.964 - 1.193   1.173    2567    1154
    4   10.4  0.1465   0.922 - 1.052   0.916 - 1.119   1.111    4179    2121
    5  -10.4  0.1481   0.589 - 0.687   0.960 - 1.083   1.093    2965    1526
    6  -10.4  0.1323   0.962 - 1.083   0.837 - 1.243   1.106    4344    2327
Ratio of minimum to maximum apparent transmission: 0.673518

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   pyrrCA h2o rmT  
  Formula   C5H6O3N1  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.22 x 0.1 x 0.06 (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    'graphite'
_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/