EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2006src0966

Report generated Aug 09, 2006; 08:09:50

Unit cell

4117 reflections with 1.00°<theta<26.02° (resolution between 20.40A and 0.81A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)9.4791 +/- 0.0003
b (Angstrom)10.2283 +/- 0.0002
c (Angstrom)11.4144 +/- 0.0003
alpha (°)88.4231 +/- 0.0015
beta (°)78.1711 +/- 0.0016
gamma (°)79.6936 +/- 0.0016
Volume (A**3)1065.66 +/- 0.05
Mosaicity (°)0.607 +/- 0.002

Data collection

Summary

Total number of images collected239
Total exposure time231.5 minutes
Data collection exposure time229.8 minutes
Data collection wall-clock time253.7 minutes

Experimental Conditions

Wavelength0.71073 A

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Detector
distance		Used in
scaling
cell determinationi01f10 10.0° phi1.000°10 seconds45.00 mmNo
data collections01f54108.0° omega2.000°60 seconds30.00 mmYes
data collections02f47 94.0° omega2.000°60 seconds30.00 mmYes
data collections03f21 42.0° omega2.000°60 seconds30.00 mmYes
data collections04f54108.0° omega2.000°60 seconds30.00 mmYes
data collections05f53106.0° omega2.000°60 seconds30.00 mmYes

Scalepack Scaling

Deleted observations

Rejected  39
Overload or incomplete profile 442
Sigma cutoff   9
High resolution limit  20

Final Data Set

Scale factor range9.33-10.13
Number of 'full' reflections 10266
Number of 'partial' reflections  7718
Total number of integrated reflections 17289
Total number of unique reflections  4192
Data completeness  99.8%
Resolution range20.40-0.81 A
Theta range1.00°-26.02°
Average Intensity  193.3
Average Sigma(I)    4.7
Overall R-merge (linear)  0.026

Sadabs Results

Parameter refinement on 13951 reflections reduced R(int) from 0.0480 to 0.0237

Before rejection, 16730 reflections total and 4200 unique

After rejection, 16631 reflections total and 4193 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   -3.7  0.0259   0.834 - 0.923   0.973 - 1.050   1.109    3956    3436
    2   -3.8  0.0244   1.016 - 1.104   0.973 - 1.054   1.118    3416    2981
    3   -4.0  0.0222   0.972 - 1.021   0.956 - 1.028   1.130    1418    1239
    4   -3.8  0.0241   0.937 - 1.013   0.956 - 1.098   1.144    3971    3477
    5   -3.8  0.0255   1.004 - 1.069   0.976 - 1.060   1.116    3870    3371
Ratio of minimum to maximum apparent transmission: 0.870933

Metadata

  Group    Academic  
  Operator   Susanne Huth  
  Sample Owner   Robert Shaw  
  Local Code   0172054  
  Formula   C4H4N5Cl4P3  
  Crystal Colour   Clear Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.28 x 0.21 x 0.14 (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/