EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0237r

Report generated Jun 21, 2007; 08:16:27

Unit cell

55769 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)10.72290 +/- 0.00010
b (Angstrom)10.23950 +/- 0.00010
c (Angstrom)20.1530 +/- 0.0002
alpha (°) 90.000
beta (°)92.7121 +/- 0.0007
gamma (°) 90.000
Volume (A**3)2210.26 +/- 0.04
Mosaicity (°)0.4880 +/- 0.0010

Data collection

Summary

Total number of images collected763
Total exposure time10.6 hours
Data collection exposure time10.6 hours
Data collection wall-clock time11.1 hours

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 collections01f363363.0° phi1.000°50 secondsYes
data collections02f27 27.0° omega1.000°50 secondsYes
data collections03f27 27.0° omega1.000°50 secondsYes
data collections04f111111.0° omega1.000°50 secondsYes
data collections05f55 55.0° omega1.000°50 secondsYes
data collections06f61 61.0° omega1.000°50 secondsYes
data collections07f111111.0° omega1.000°50 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   6
Zero sigma or profile test   7
Overload or incomplete profile1916
Sigma cutoff 398
Low resolution limit   1
High resolution limit 118

Final Data Set

Scale factor10.00
Number of 'full' reflections 16201
Number of 'partial' reflections 28989
Total number of integrated reflections 42194
Total number of unique reflections  5318
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  425.4
Average Sigma(I)    6.0
Overall R-merge (linear)  0.166

Sadabs Results

Parameter refinement on 37920 reflections reduced R(int) from 0.1173 to 0.0347

Before rejection, 42993 reflections total and 5341 unique

After rejection, 40002 reflections total and 5338 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.1  0.0412   0.864 - 1.638   0.984 - 1.050   2.510   19169   16520
    2   14.6  0.0288   0.813 - 1.052   0.993 - 1.042   2.299    1356    1171
    3   14.6  0.0287   0.699 - 0.826   1.005 - 1.046   2.318    1348    1180
    4   14.6  0.0284   0.779 - 1.078   0.984 - 1.029   2.256    5952    5175
    5   14.6  0.0268   0.766 - 0.964   1.005 - 1.045   2.248    2933    2566
    6   14.6  0.0261   0.537 - 0.628   0.986 - 1.052   2.165    3220    2811
    7   14.6  0.0268   0.627 - 0.722   0.987 - 1.036   2.242    6024    5355
Ratio of minimum to maximum apparent transmission: 0.934560

Metadata

  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr P. G. Taylor  
  Local Code   SM Exp 10A  
  Formula   C21 H36 N2 O2 Si2  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.16 x 0.1 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 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/