EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2007src0256

Report generated Feb 23, 2007; 15:12:31

Unit cell

56688 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)9.5626 +/- 0.0004
b (Angstrom)10.5996 +/- 0.0006
c (Angstrom)19.5666 +/- 0.0011
alpha (°)91.038 +/- 0.003
beta (°)90.726 +/- 0.003
gamma (°)90.039 +/- 0.004
Volume (A**3)1982.78 +/- 0.18
Mosaicity (°)1.772 +/- 0.003

Data collection

Summary

Total number of images collected356
Total exposure time71.5 minutes
Data collection exposure time70.8 minutes
Data collection wall-clock time99.9 minutes

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°12 secondsYes
data collections02f17 34.0° omega2.000°12 secondsYes
data collections03f26 52.0° omega2.000°12 secondsYes
data collections04f28 56.0° omega2.000°12 secondsYes
data collections05f36 72.0° omega2.000°12 secondsYes
data collections06f60120.0° omega2.000°12 secondsYes
Phi/Chii01f - i08f85 seconds

Scalepack Scaling

Deleted observations

Rejected 595
Zero sigma or profile test   7
Overload or incomplete profile1568
Sigma cutoff 122
High resolution limit  61

Final Data Set

Scale factor range9.72-12.95
Number of 'full' reflections  1180
Number of 'partial' reflections 32160
Total number of integrated reflections 21620
Total number of unique reflections  6936
Data completeness  75.6%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  107.8
Average Sigma(I)    4.5
Overall R-merge (linear)  0.050

Sadabs Results

Parameter refinement on 23146 reflections reduced R(int) from 0.1138 to 0.0612

Before rejection, 33733 reflections total and 8691 unique

After rejection, 32022 reflections total and 8655 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0594   0.830 - 1.027   0.926 - 1.342   1.365   17419   12615
    2   11.2  0.0765   0.631 - 0.734   0.973 - 1.220   1.444    1320    1004
    3    9.5  0.0795   0.819 - 0.945   0.958 - 1.213   1.471    2202    1653
    4   11.2  0.0680   0.578 - 0.741   0.927 - 1.048   1.502    2386    1682
    5   11.2  0.0547   0.850 - 1.120   0.927 - 1.176   1.417    3092    2418
    6   11.2  0.0605   0.771 - 0.961   0.951 - 1.130   1.475    5603    4170
Ratio of minimum to maximum apparent transmission: 0.690349

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Davies  
  Local Code   306-721-2  
  Formula   C18H24N5O2P3  
  Crystal Colour    Colourless  
  Crystal Habit    Slab  
  Crystal Size   0.4 x 0.2 x 0.2 (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/