EPSRC National Crystallography Service
Data Collection Summary kccd1 (dellboy)

Summary report for Directory: diska/2007src0258

Report generated Feb 22, 2007; 08:37:49

Unit cell

93378 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p4
a (Angstrom)11.50070 +/- 0.00010
b (Angstrom)11.50070 +/- 0.00010
c (Angstrom)16.78330 +/- 0.00010
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)2219.86 +/- 0.03
Mosaicity (°)0.5950 +/- 0.0010

Data collection

Summary

Total number of images collected733
Total exposure time12.1 hours
Data collection exposure time12.1 hours
Data collection wall-clock time13.2 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance30.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f363363.0° phi1.000°60 secondsYes
data collections02f34 34.0° omega1.000°60 secondsYes
data collections03f34 34.0° omega1.000°60 secondsYes
data collections04f110110.0° omega1.000°60 secondsYes
data collections05f46 46.0° omega1.000°60 secondsYes
data collections06f46 46.0° omega1.000°60 secondsYes
data collections07f46 46.0° omega1.000°60 secondsYes
data collections08f46 46.0° omega1.000°60 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected 341
Zero sigma or profile test   6
Overload or incomplete profile1764
Sigma cutoff  92
High resolution limit  38

Final Data Set

Scale factor range9.70-19.60
Number of 'full' reflections 14875
Number of 'partial' reflections 44806
Total number of integrated reflections 55531
Total number of unique reflections  2634
Data completeness 100.0%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  151.4
Average Sigma(I)    2.0
Overall R-merge (linear)  0.045

Sadabs Results

Parameter refinement on 52423 reflections reduced R(int) from 0.1088 to 0.0424

Before rejection, 57423 reflections total and 2645 unique

After rejection, 56868 reflections total and 2644 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    7.4  0.0434   1.333 - 1.496   0.936 - 1.124   1.348   28737   26397
    2    6.8  0.0422   0.585 - 0.721   0.959 - 1.049   1.236    2561    2395
    3    6.8  0.0472   0.620 - 0.792   0.919 - 1.069   1.283    2579    2417
    4    6.8  0.0422   0.494 - 0.935   0.919 - 1.078   1.233    8744    8263
    5    6.8  0.0472   0.510 - 0.696   0.919 - 1.087   1.234    3544    3314
    6    6.8  0.0445   0.591 - 0.703   0.919 - 1.141   1.201    3572    3320
    7    6.8  0.0429   0.584 - 0.703   0.919 - 1.141   1.211    3562    3327
    8    6.8  0.0437   0.589 - 0.702   0.919 - 1.133   1.202    3569    3338
Ratio of minimum to maximum apparent transmission: 0.805074

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Davies  
  Local Code   306-725-1  
  Formula   C18H24N5O2P3S2  
  Crystal Colour    Colourless  
  Crystal Habit    Rod  
  Crystal Size   0.6 x 0.05 x 0.02 (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/