EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2005slh0414

Report generated May 09, 2005; 08:05:54

Unit cell

3477 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)8.11860 +/- 0.00010
b (Angstrom)17.6096 +/- 0.0002
c (Angstrom)10.39750 +/- 0.00010
alpha (°) 90.000
beta (°)100.5223 +/- 0.0008
gamma (°) 90.000
Volume (A**3)1461.48 +/- 0.03
Mosaicity (°)0.3710 +/- 0.0010

Data collection

Summary

Total number of images collected638
Total exposure time11.5 hours
Data collection exposure time11.4 hours
Data collection wall-clock time12.4 hours

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 collections01f242242.0° phi1.000°65 secondsYes
data collections02f32 32.0° omega1.000°65 secondsYes
data collections03f46 46.0° omega1.000°65 secondsYes
data collections04f103103.0° omega1.000°65 secondsYes
data collections05f110110.0° omega1.000°65 secondsYes
data collections06f97 97.0° omega1.000°65 secondsYes
Phi/Chii01f - i08f830 seconds

Scalepack Scaling

Deleted observations

Rejected 258
Zero sigma or profile test   7
Overload or incomplete profile 778
Sigma cutoff  12
High resolution limit   9

Final Data Set

Scale factor range9.26-10.01
Number of 'full' reflections 16574
Number of 'partial' reflections 17296
Total number of integrated reflections 32437
Total number of unique reflections  3481
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   75.2
Average Sigma(I)    1.7
Overall R-merge (linear)  0.037

Sadabs Results

Parameter refinement on 25432 reflections reduced R(int) from 0.0759 to 0.0337

Before rejection, 32905 reflections total and 3484 unique

After rejection, 32601 reflections total and 3480 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0355   0.929 - 1.062   0.980 - 1.110   1.098   12633   10344
    2   -6.8  0.0370   0.501 - 0.533   0.984 - 1.058   1.085    1568    1267
    3   -6.8  0.0391   0.886 - 0.939   0.984 - 1.069   1.057    2330    1884
    4   -6.8  0.0353   0.930 - 1.020   0.978 - 1.115   1.049    5348    4419
    5   -6.8  0.0358   1.616 - 1.781   0.984 - 1.052   1.103    5705    4595
    6   -6.8  0.0367   0.681 - 0.747   0.978 - 1.061   1.043    5017    4153
Ratio of minimum to maximum apparent transmission: 0.876968

Metadata

  Group    Mike Hursthouse  
  Operator   Susanne Huth  
  Sample Owner     
  Local Code   CAG 143  
  Formula   C26 H28 N2 O4 P2 S4 Cd1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.12 x 0.06 x 0.06 (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/