EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0060

Report generated Jan 26, 2009; 13:20:41

Unit cell

30099 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)7.2549 +/- 0.0002
b (Angstrom)8.1109 +/- 0.0002
c (Angstrom)16.9313 +/- 0.0004
alpha (°)80.4084 +/- 0.0014
beta (°)78.6807 +/- 0.0014
gamma (°)89.6743 +/- 0.0014
Volume (A**3)962.89 +/- 0.04
Mosaicity (°)0.758 +/- 0.002

Data collection

Summary

Total number of images collected488
Total exposure time63.7 minutes
Data collection exposure time62.6 minutes
Data collection wall-clock time82.7 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f68102.0° omega1.500°7 secondsYes
data collections02f57 85.5° omega1.500°7 secondsYes
data collections03f68102.0° omega1.500°7 secondsYes
data collections04f46 69.0° omega1.500°7 secondsYes
data collections05f46 69.0° omega1.500°7 secondsYes
data collections06f64 96.0° omega1.500°7 secondsYes
data collections07f67100.5° omega1.500°7 secondsYes
data collections08f64 96.0° omega1.500°7 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test  10
Overload or incomplete profile 780
Sigma cutoff 202
High resolution limit  18

Final Data Set

Scale factor10.00
Number of 'full' reflections  7664
Number of 'partial' reflections 15711
Total number of integrated reflections 21500
Total number of unique reflections  4424
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   84.1
Average Sigma(I)    2.3
Overall R-merge (linear)  0.229

Sadabs Results

Parameter refinement on 18630 reflections reduced R(int) from 0.1493 to 0.0627

Before rejection, 21889 reflections total and 4432 unique

After rejection, 19709 reflections total and 4422 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    6.7  0.0617   0.564 - 1.030   0.931 - 1.158   2.073    2875    2506
    2   10.0  0.0569   0.574 - 0.745   0.936 - 1.158   2.042    2342    2030
    3    8.3  0.0590   0.671 - 1.252   0.967 - 1.207   2.033    2859    2383
    4   10.2  0.0531   0.650 - 0.754   0.936 - 1.158   2.053    1863    1626
    5   10.2  0.0525   0.908 - 1.218   0.955 - 1.158   2.059    1841    1578
    6   10.2  0.0746   0.700 - 1.641   0.956 - 1.231   2.251    2552    1969
    7   10.2  0.0624   0.853 - 1.155   0.933 - 1.144   2.100    2744    2267
    8   10.2  0.0550   0.706 - 0.856   0.936 - 1.132   2.043    2633    2268
Ratio of minimum to maximum apparent transmission: 0.756863

Metadata

  Group    Service  
  Operator   Sam Callear  
  Sample Owner   Dr A Fogg  
  Local Code   JN51  
  Formula   C10H8O11S2La2W2  
  Crystal Colour    Colourless  
  Crystal Habit    Blade  
  Crystal Size   0.14 x 0.03 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 2007/2 (Sheldrick, G.M., 2007)'

_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 APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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. (2007). SADABS. Version 2007/2. 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/