EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src1135

Report generated Nov 25, 2009; 08:56:53

Unit cell

64578 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p2
a (Angstrom)10.4550 +/- 0.0004
b (Angstrom)14.6532 +/- 0.0008
c (Angstrom)18.1135 +/- 0.0010
alpha (°) 90.000
beta (°)94.095 +/- 0.002
gamma (°) 90.000
Volume (A**3)2767.9 +/- 0.2
Mosaicity (°)1.0110 +/- 0.0010

Data collection

Summary

Total number of images collected579
Total exposure time12.8 hours
Data collection exposure time12.7 hours
Data collection wall-clock time13.1 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance49.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f362362.0° phi1.000°80 secondsYes
data collections02f27 27.0° omega1.000°80 secondsYes
data collections03f74 74.0° omega1.000°80 secondsYes
data collections04f27 27.0° omega1.000°80 secondsYes
data collections05f47 47.0° omega1.000°80 secondsYes
data collections06f34 34.0° omega1.000°80 secondsYes
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Rejected   1
Zero sigma or profile test   9
Overload or incomplete profile 530
Sigma cutoff 552
High resolution limit 256

Final Data Set

Scale factor10.00
Number of 'full' reflections     0
Number of 'partial' reflections 30117
Total number of integrated reflections 27801
Total number of unique reflections  6532
Data completeness  99.8%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity  106.7
Average Sigma(I)    3.1
Overall R-merge (linear)  0.089

Sadabs Results

Parameter refinement on 22759 reflections reduced R(int) from 0.0729 to 0.0465

Before rejection, 28653 reflections total and 6594 unique

After rejection, 25224 reflections total and 6576 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   24.2  0.0476   0.936 - 1.250   0.977 - 1.124   2.065   16250   12821
    2   23.6  0.0576   0.351 - 0.404   0.993 - 1.119   2.165    1109     827
    3   23.6  0.0544   0.830 - 1.038   0.995 - 1.304   2.084    3309    2566
    4   23.6  0.0605   0.323 - 0.385   0.997 - 1.101   2.125    1071     812
    5   23.6  0.0488   0.849 - 1.124   0.997 - 1.104   2.045    2065    1606
    6   23.6  0.0477   0.549 - 0.635   0.977 - 1.103   1.992    1420    1151
Ratio of minimum to maximum apparent transmission: 0.749329

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr L Martin  
  Local Code   LeeSnitromethane  
  Formula   C37 H27 N O14 Na Cr  
  Crystal Colour    Dark Orange  
  Crystal Habit    Sheet  
  Crystal Size   0.08 x 0.05 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/