EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src0769

Report generated Jun 27, 2007; 16:18:10

Unit cell

10676 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)8.8971 +/- 0.0004
b (Angstrom)9.5970 +/- 0.0004
c (Angstrom)9.8882 +/- 0.0003
alpha (°)64.918 +/- 0.002
beta (°)81.546 +/- 0.002
gamma (°)68.435 +/- 0.002
Volume (A**3)711.13 +/- 0.05
Mosaicity (°)0.593 +/- 0.002

Data collection

Summary

Total number of images collected328
Total exposure time87.8 minutes
Data collection exposure time87.0 minutes
Data collection wall-clock time101.9 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance31.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°16 secondsYes
data collections02f13 26.0° omega2.000°16 secondsYes
data collections03f13 26.0° omega2.000°16 secondsYes
data collections04f52104.0° omega2.000°16 secondsYes
data collections05f24 48.0° omega2.000°16 secondsYes
data collections06f24 48.0° omega2.000°16 secondsYes
data collections07f13 26.0° omega2.000°16 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Overload or incomplete profile 384
Sigma cutoff 159
High resolution limit  93

Final Data Set

Scale factor10.00
Number of 'full' reflections  8215
Number of 'partial' reflections  6099
Total number of integrated reflections 13432
Total number of unique reflections  3227
Data completeness  99.7%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   77.9
Average Sigma(I)    2.2
Overall R-merge (linear)  0.093

Sadabs Results

Parameter refinement on 10031 reflections reduced R(int) from 0.0877 to 0.0470

Before rejection, 13319 reflections total and 3268 unique

After rejection, 11965 reflections total and 3252 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.7  0.0512   1.055 - 1.480   0.966 - 1.137   2.098    6971    5203
    2   11.1  0.0463   0.498 - 0.559   0.977 - 1.072   2.071     418     321
    3   11.1  0.0433   0.508 - 0.566   1.012 - 1.088   2.004     422     309
    4   11.1  0.0461   0.642 - 0.914   0.982 - 1.088   2.049    1991    1504
    5   11.1  0.0466   0.532 - 0.614   0.977 - 1.082   2.080     883     666
    6   11.1  0.0453   0.706 - 0.853   1.004 - 1.106   2.088     851     617
    7   11.1  0.0457   0.547 - 0.575   0.983 - 1.069   2.092     429     331
Ratio of minimum to maximum apparent transmission: 0.849863

Metadata

  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr Peter Taylor  
  Local Code   PoC 1(d)  
  Formula   C17 H35 N2 O3  
  Crystal Colour    Colourless  
  Crystal Habit    Block  
  Crystal Size   0.22 x 0.12 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/