EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/05skc0002

Report generated Feb 16, 2005; 07:48:13

Unit cell

880 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)5.1603 +/- 0.0003
b (Angstrom)5.3269 +/- 0.0002
c (Angstrom)7.5265 +/- 0.0004
alpha (°)78.737 +/- 0.003
beta (°)83.327 +/- 0.003
gamma (°)79.095 +/- 0.003
Volume (A**3)198.567 +/- 0.018
Mosaicity (°)0.429 +/- 0.003

Data collection

Summary

Total number of images collected346
Total exposure time13.3 hours
Data collection exposure time13.2 hours
Data collection wall-clock time13.7 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance32.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f136272.0° phi2.000°140 secondsYes
data collections02f16 32.0° omega2.000°140 secondsYes
data collections03f56112.0° omega2.000°140 secondsYes
data collections04f25 50.0° omega2.000°140 secondsYes
data collections05f53106.0° omega2.000°140 secondsYes
data collections06f52104.0° omega2.000°140 secondsYes
Phi/Chii01f - i08f860 seconds

Scalepack Scaling

Deleted observations

Rejected  20
Zero sigma or profile test   2
Overload or incomplete profile 104
Sigma cutoff   1
High resolution limit  22

Final Data Set

Scale factor range9.68-10.12
Number of 'full' reflections  3148
Number of 'partial' reflections  1410
Total number of integrated reflections  4336
Total number of unique reflections   898
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   64.9
Average Sigma(I)    2.0
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 3813 reflections reduced R(int) from 0.0509 to 0.0357

Before rejection, 4355 reflections total and 911 unique

After rejection, 4317 reflections total and 910 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    9.3  0.0368   0.952 - 1.053   0.964 - 1.097   1.149    1781    1637
    2   -8.7  0.0342   0.801 - 0.845   0.957 - 1.037   1.048     183     169
    3   -8.7  0.0349   0.980 - 1.079   0.960 - 1.059   1.102     716     661
    4   -8.7  0.0364   0.839 - 0.906   0.976 - 1.042   1.096     305     275
    5   -8.7  0.0345   0.751 - 0.850   0.970 - 1.053   1.108     675     625
    6   -8.7  0.0422   0.952 - 1.023   0.957 - 1.038   1.151     657     603
Ratio of minimum to maximum apparent transmission: 0.872067

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear (skc)  
  Sample Owner     
  Local Code   TLT374B GH12  
  Formula   C5O6N1H11  
  Crystal Colour    Colourless  
  Crystal Habit    Fragment  
  Crystal Size   0.2 x 0.12 x 0.02 (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  'BrukerNonius 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/