EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2006src1374

Report generated Dec 05, 2006; 16:02:54

Unit cell

4105 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p222
a (Angstrom)7.8607 +/- 0.0003
b (Angstrom)19.6225 +/- 0.0012
c (Angstrom)21.4010 +/- 0.0012
alpha (°) 90.000
beta (°) 90.000
gamma (°) 90.000
Volume (A**3)3301.0 +/- 0.3
Mosaicity (°)1.020 +/- 0.002

Data collection

Summary

Total number of images collected383
Total exposure time12.6 hours
Data collection exposure time12.5 hours
Data collection wall-clock time12.8 hours

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance42.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f99158.4° phi1.600°120 secondsYes
data collections02f41 65.6° omega1.600°120 secondsNo
data collections03f73116.8° omega1.600°120 secondsYes
data collections04f73116.8° omega1.600°120 secondsYes
data collections05f73116.8° omega1.600°120 secondsYes
data collections06f16 25.6° omega1.600°120 secondsNo
Phi/Chii01f - i08f840 seconds

Scalepack Scaling

Deleted observations

Rejected1290
Zero sigma or profile test  55
Overload or incomplete profile1420
Sigma cutoff1172
High resolution limit  40

Final Data Set

Scale factor range5.57-27.50
Number of 'full' reflections  8117
Number of 'partial' reflections 27912
Total number of integrated reflections 31005
Total number of unique reflections  4205
Data completeness  98.1%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   13.8
Average Sigma(I)    0.8
Overall R-merge (linear)  0.172

Eval Integration

Number of reflections 42860
Unique reflections  8771
Weak reflections 17993
Negative intensities  2421
R-sym 0.499
R-meas 0.529

Sadabs Results

Parameter refinement on 19154 reflections reduced R(int) from 0.2526 to 0.1054

Before rejection, 35009 reflections total and 4249 unique

After rejection, 28729 reflections total and 4233 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   20.2  0.1978   0.606 - 0.882   0.905 - 1.274   2.134    9055    3500
    2   16.7  0.1694   0.525 - 1.725   0.895 - 1.336   2.087    6666    2897
    3  -19.6  0.0831   0.559 - 0.811   0.895 - 1.167   1.788    6757    4069
    4   11.5  0.1110   0.588 - 0.735   0.996 - 1.279   1.989    6251    3565

Sadabs Results

Parameter refinement on 11301 reflections reduced R(int) from 0.2422 to 0.1078

Before rejection, 27752 reflections total and 7262 unique

After rejection, 25399 reflections total and 7259 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -20.2  0.2459   0.865 - 1.308   0.885 - 1.401   1.923    6793    2442
    2  -19.6  0.4820   1.209 - 2.376   1.065 - 2.043   1.988    3016     698
    3  -16.7  0.2185   0.535 - 1.716   0.757 - 1.860   1.846    5617    2181
    4   19.6  0.1051   0.445 - 0.587   0.761 - 1.382   1.544    4728    2707
    5  -11.5  0.1494   0.528 - 0.668   0.971 - 1.642   1.755    4554    2352
    6  -19.6  0.2849   1.966 - 2.255   0.784 - 1.246   1.906     691     208
Ratio of minimum to maximum apparent transmission: 0.669862

Metadata

  Group    Service  
  Operator   Louise Male  
  Sample Owner   Dr S. Aldridge  
  Local Code   JK0137_b  
  Formula   C46 H50 O8 B4 Fe3  
  Crystal Colour    Brown  
  Crystal Habit    Plate  
  Crystal Size   0.19 x 0.04 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 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    '10cm confocal mirrors'
_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/