EPSRC National Crystallography Service

Data Collection Summary kccd1 (dellboy)

 

Summary report for Directory: diska/2009src0460

Report generated Apr 27, 2009; 11:35:34

Unit cell

14061 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)

6.1704 +/- 0.0004

b (Angstrom)

7.1051 +/- 0.0005

c (Angstrom)

10.8713 +/- 0.0006

alpha (°)

79.486 +/- 0.004

beta (°)

76.174 +/- 0.004

gamma (°)

67.853 +/- 0.003

Volume (A**3)

426.39 +/- 0.05

Mosaicity (°)

1.144 +/- 0.004

Data collection

Summary

Total number of images collected

333

Total exposure time

111.2 minutes

Data collection exposure time

109.5 minutes

Data collection wall-clock time

142.0 minutes

Experimental Conditions

Wavelength

0.71073 A

Crystal to detector distance

30.00 mm

Scans

Type

Name

# images

Total
Rotation

Per frame
Rotation

Exposure
per frame

Used in
scaling

data collection

s01f

179

358.0° phi

2.000°

20 seconds

Yes

data collection

s02f

17

 34.0° omega

2.000°

20 seconds

Yes

data collection

s03f

55

110.0° omega

2.000°

20 seconds

Yes

data collection

s04f

23

 46.0° omega

2.000°

20 seconds

Yes

data collection

s05f

51

102.0° omega

2.000°

20 seconds

Yes

Phi/Chi

i01f - i08f

8

12 seconds

Scalepack Scaling

Deleted observations

Rejected

  21

Zero sigma or profile test

   2

Overload or incomplete profile

 312

Sigma cutoff

   6

High resolution limit

 106

Final Data Set

Scale factor

10.00

Number of 'full' reflections

  2819

Number of 'partial' reflections

  7518

Total number of integrated reflections

  9740

Total number of unique reflections

  1931

Data completeness

  99.8%

Resolution range

7.00-0.77 A

Theta range

2.91°-27.48°

Average Intensity

   75.9

Average Sigma(I)

    2.4

Overall R-merge (linear)

  0.070

Sadabs Results

Estimated minimum and maximum transmission: 0.6657 0.7456

Metadata

  Group  

 Service  

  Operator  

 Sam Callear  

  Sample Owner  

 Dr J Spencer  

  Local Code  

 HP158 

  Formula  

 C8H5N3O 

  Crystal Colour  

  Colourless  

  Crystal Habit  

  Plate  

  Crystal Size  

 0.23 x 0.2 x 0.06 (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    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper 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. (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/