EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)


Summary report for Directory: diska/2007src0203

Report generated Feb 27, 2007; 08:54:41

Unit cell

23814 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)10.2222 +/- 0.0002
b (Angstrom)12.4363 +/- 0.0003
c (Angstrom)19.6192 +/- 0.0005
alpha (°)83.7804 +/- 0.0013
beta (°)86.1256 +/- 0.0015
gamma (°)77.7912 +/- 0.0013
Volume (A**3)2420.80 +/- 0.10
Mosaicity (°)0.4340 +/- 0.0010

Data collection

Summary

Total number of images collected340
Total exposure time13.0 hours
Data collection exposure time12.9 hours
Data collection wall-clock time13.5 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 collections01f181362.0° phi2.000°140 secondsYes
data collections02f17 34.0° omega2.000°140 secondsYes
data collections03f16 32.0° omega2.000°140 secondsYes
data collections04f28 56.0° omega2.000°140 secondsYes
data collections05f60120.0° omega2.000°140 secondsYes
data collections06f30 60.0° omega2.000°140 secondsYes
Phi/Chii01f - i08f820 seconds

Scalepack Scaling

Deleted observations

Rejected 897
Zero sigma or profile test 324
Overload or incomplete profile 820
Sigma cutoff 230
High resolution limit  57

Final Data Set

Scale factor range6.00-10.28
Number of 'full' reflections 32991
Number of 'partial' reflections 14997
Total number of integrated reflections 45027
Total number of unique reflections 11064
Data completeness  99.9%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   33.3
Average Sigma(I)    1.8
Overall R-merge (linear)  0.068

Sadabs Results

Parameter refinement on 29333 reflections reduced R(int) from 0.0978 to 0.0512

Before rejection, 46264 reflections total and 11106 unique

After rejection, 45290 reflections total and 11102 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0628   0.871 - 0.944   0.966 - 1.210   1.245   25330   18045
    2   11.2  0.0760   0.909 - 0.972   0.983 - 1.217   1.305    2191    1490
    3   11.2  0.0864   0.721 - 0.784   0.973 - 1.130   1.389    1410     859
    4   11.2  0.0694   0.899 - 0.951   0.977 - 1.240   1.264    3810    2638
    5   11.2  0.0651   0.865 - 0.952   0.966 - 1.274   1.272    8463    5941
    6   11.2  0.0676   0.909 - 0.971   0.966 - 1.322   1.287    4086    2850
Ratio of minimum to maximum apparent transmission: 0.731017

Metadata

  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr Alan Kennedy  
  Local Code   CuH6AE1  
  Formula   C36 H57 S3 N5 O3 Cu1  
  Crystal Colour    Pale Blue  
  Crystal Habit    Slab  
  Crystal Size   0.16 x 0.16 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/