EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/05src0132

Report generated Feb 01, 2005; 16:39:54

Unit cell

9529 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)12.9601 +/- 0.0002
b (Angstrom)13.1010 +/- 0.0002
c (Angstrom)14.6744 +/- 0.0002
alpha (°)79.7603 +/- 0.0008
beta (°)80.9361 +/- 0.0009
gamma (°)61.8059 +/- 0.0007
Volume (A**3)2153.19 +/- 0.06
Mosaicity (°)0.5690 +/- 0.0010

Data collection

Summary

Total number of images collected621
Total exposure time84.6 minutes
Data collection exposure time83.9 minutes
Data collection wall-clock time133.8 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 collections01f363363.0° phi1.000°8 secondsYes
data collections02f34 34.0° omega1.000°8 secondsYes
data collections03f34 34.0° omega1.000°8 secondsYes
data collections04f63 63.0° omega1.000°8 secondsYes
data collections05f46 46.0° omega1.000°8 secondsYes
data collections06f73 73.0° omega1.000°8 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 215
Zero sigma or profile test  12
Overload or incomplete profile1918
Sigma cutoff  28
High resolution limit  18

Final Data Set

Scale factor range9.89-11.43
Number of 'full' reflections 13408
Number of 'partial' reflections 34963
Total number of integrated reflections 43929
Total number of unique reflections  9827
Data completeness  99.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  114.2
Average Sigma(I)    2.9
Overall R-merge (linear)  0.028

Sadabs Results

Parameter refinement on 37467 reflections reduced R(int) from 0.0675 to 0.0273

Before rejection, 46661 reflections total and 9851 unique

After rejection, 46171 reflections total and 9840 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0273   0.955 - 1.167   0.961 - 1.117   1.361   27830   22950
    2   -6.8  0.0274   0.665 - 0.699   0.966 - 1.082   1.324    2417    2012
    3   -6.8  0.0252   0.661 - 0.723   0.948 - 1.059   1.317    2423    2016
    4   -6.8  0.0293   0.973 - 1.025   0.948 - 1.079   1.360    4688    3889
    5   -6.8  0.0320   0.703 - 0.757   0.954 - 1.107   1.418    3370    2774
    6   -6.8  0.0280   0.904 - 0.964   0.948 - 1.091   1.337    5443    4499
Ratio of minimum to maximum apparent transmission: 0.848787

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Lancaster  
  Local Code   AM467  
  Formula   C42H43B2F15LiO3P  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.45 x 0.2 x 0.18 (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/