EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2005src0300

Report generated Apr 01, 2005; 12:21:01

Unit cell

9025 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)12.2610 +/- 0.0003
b (Angstrom)12.2997 +/- 0.0002
c (Angstrom)14.6002 +/- 0.0003
alpha (°)84.9816 +/- 0.0013
beta (°)71.2502 +/- 0.0013
gamma (°)73.5675 +/- 0.0014
Volume (A**3)1999.78 +/- 0.07
Mosaicity (°)0.8520 +/- 0.0010

Data collection

Summary

Total number of images collected321
Total exposure time105.8 minutes
Data collection exposure time105.5 minutes
Data collection wall-clock time132.5 minutes

Experimental Conditions

Wavelength0.71073 A
Cryostat setting125.00K
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°20 secondsYes
data collections02f17 34.0° omega2.000°20 secondsYes
data collections03f16 32.0° omega2.000°20 secondsYes
data collections04f54108.0° omega2.000°20 secondsYes
data collections05f23 46.0° omega2.000°20 secondsYes
data collections06f22 44.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f82 seconds

Scalepack Scaling

Deleted observations

Rejected 227
Overload or incomplete profile2000
Sigma cutoff  66
High resolution limit 123

Final Data Set

Scale factor range8.39-31.34
Number of 'full' reflections 19287
Number of 'partial' reflections 26976
Total number of integrated reflections 43226
Total number of unique reflections  9147
Data completeness  99.4%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  183.2
Average Sigma(I)    4.7
Overall R-merge (linear)  0.051

Sadabs Results

Parameter refinement on 33629 reflections reduced R(int) from 0.3227 to 0.0639

Before rejection, 42904 reflections total and 9228 unique

After rejection, 41305 reflections total and 9184 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0538   0.734 - 1.767   0.923 - 1.237   1.407   24751   19996
    2   -5.8  0.0657   0.204 - 0.230   0.926 - 1.149   1.435    1966    1611
    3   -6.8  0.0629   0.538 - 0.671   0.971 - 1.198   1.469    1963    1511
    4   -6.8  0.0970   0.447 - 0.720   0.925 - 1.234   1.810    6884    5368
    5   -6.8  0.0644   0.640 - 0.772   0.926 - 1.157   1.418    2960    2402
    6   -6.8  0.0550   0.657 - 0.740   0.924 - 1.089   1.367    2781    2256
Ratio of minimum to maximum apparent transmission: 0.745935

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Lancaster  
  Local Code   AM492  
  Formula   C46H53ALBF15LiO4P  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.5 x 0.2 x 0.2 (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/