EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/06skc0067

Report generated Jan 19, 2007; 14:07:16

Unit cell

6633 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)8.1621 +/- 0.0006
b (Angstrom)9.3259 +/- 0.0005
c (Angstrom)21.3026 +/- 0.0012
alpha (°)86.922 +/- 0.004
beta (°)88.863 +/- 0.003
gamma (°)87.350 +/- 0.004
Volume (A**3)1617.21 +/- 0.17
Mosaicity (°)1.524 +/- 0.003

Data collection

Summary

Total number of images collected495
Total exposure time265.0 minutes
Data collection exposure time262.3 minutes
Data collection wall-clock time288.8 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance35.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f226361.6° phi1.600°32 secondsYes
data collections02f16 25.6° omega1.600°32 secondsYes
data collections03f34 54.4° omega1.600°32 secondsYes
data collections04f34 54.4° omega1.600°32 secondsYes
data collections05f38 60.8° omega1.600°32 secondsYes
data collections06f34 54.4° omega1.600°32 secondsYes
data collections07f36 57.6° omega1.600°32 secondsYes
data collections08f69110.4° omega1.600°32 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 820
Zero sigma or profile test  27
Overload or incomplete profile 962
Sigma cutoff1142
High resolution limit 198

Final Data Set

Scale factor range8.69-12.69
Number of 'full' reflections   343
Number of 'partial' reflections 32542
Total number of integrated reflections 26866
Total number of unique reflections  7313
Data completeness  98.3%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   22.8
Average Sigma(I)    1.5
Overall R-merge (linear)  0.111

Sadabs Results

Parameter refinement on 19185 reflections reduced R(int) from 0.1454 to 0.0850

Before rejection, 31521 reflections total and 7461 unique

After rejection, 27039 reflections total and 7410 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.1005   0.867 - 1.227   0.971 - 1.254   2.043   12817    7672
    2   14.6  0.1053   0.440 - 0.489   0.996 - 1.182   2.099     796     436
    3   14.6  0.1218   0.566 - 0.672   0.982 - 1.188   2.174    1814     932
    4   14.6  0.1084   0.576 - 0.697   0.993 - 1.192   2.140    1811     945
    5   14.6  0.0946   0.473 - 0.584   0.986 - 1.205   2.022    2003    1221
    6   14.6  0.1079   0.688 - 0.816   0.971 - 1.166   2.072    1865     997
    7   14.6  0.1130   0.690 - 0.841   0.968 - 1.268   1.990    2006    1190
    8   14.6  0.0859   0.854 - 1.216   0.970 - 1.296   1.894    3927    2548
Ratio of minimum to maximum apparent transmission: 0.747214

Metadata

  Group    Mike Hursthouse  
  Operator   Sam Callear  
  Sample Owner     
  Local Code   wp14 a8  
  Formula   C6H11O5N1  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.12 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/