EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: home/diska/2007src1142

Report generated Aug 20, 2007; 15:48:19

Unit cell

58258 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)9.6107 +/- 0.0003
b (Angstrom)13.1064 +/- 0.0003
c (Angstrom)13.7556 +/- 0.0004
alpha (°)95.9447 +/- 0.0017
beta (°)108.6669 +/- 0.0014
gamma (°)103.6696 +/- 0.0018
Volume (A**3)1564.52 +/- 0.08
Mosaicity (°)1.161 +/- 0.002

Data collection

Summary

Total number of images collected389
Total exposure time130.4 minutes
Data collection exposure time129.0 minutes
Data collection wall-clock time148.8 minutes

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 collections01f50100.0° omega2.000°20 secondsYes
data collections02f51102.0° omega2.000°20 secondsYes
data collections03f51102.0° omega2.000°20 secondsYes
data collections04f35 70.0° omega2.000°20 secondsYes
data collections05f51102.0° omega2.000°20 secondsYes
data collections06f50100.0° omega2.000°20 secondsYes
data collections07f45 90.0° omega2.000°20 secondsYes
data collections08f48 96.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f810 seconds

Scalepack Scaling

Deleted observations

Rejected   5
Zero sigma or profile test   1
Overload or incomplete profile1922
Sigma cutoff 858
High resolution limit   4

Final Data Set

Scale factor10.00
Number of 'full' reflections 10158
Number of 'partial' reflections 30535
Total number of integrated reflections 36771
Total number of unique reflections  7228
Data completeness  97.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  146.0
Average Sigma(I)    3.5
Overall R-merge (linear)  0.153

Sadabs Results

Parameter refinement on 29232 reflections reduced R(int) from 0.1180 to 0.0506

Before rejection, 36874 reflections total and 7242 unique

After rejection, 32823 reflections total and 7205 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    3.2  0.0510   0.577 - 1.007   0.976 - 1.111   2.091    4512    3615
    2   10.2  0.0498   0.722 - 1.048   0.940 - 1.101   2.098    4411    3556
    3   10.2  0.0536   0.989 - 1.366   0.969 - 1.108   2.164    4338    3426
    4   10.2  0.0531   0.718 - 0.920   0.996 - 1.130   2.211    2894    2217
    5   10.2  0.0484   0.752 - 1.226   0.940 - 1.071   2.057    4445    3595
    6   10.2  0.0535   0.724 - 0.920   0.966 - 1.100   2.079    4268    3220
    7   10.2  0.0554   0.830 - 1.149   0.948 - 1.129   2.170    3798    2921
    8   10.2  0.0522   0.687 - 0.845   0.968 - 1.146   2.066    4157    3186
Ratio of minimum to maximum apparent transmission: 0.820013

Metadata

  Group    Service  
  Operator   Simon Coles  
  Sample Owner   Davies  
  Local Code   307-510-4  
  Formula   C17H36N10O8P6  
  Crystal Colour    Colourless  
  Crystal Habit    Plate  
  Crystal Size   0.1 x 0.03 x 0.01 (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/