Summary report for Directory: diska/06skc0061

Report generated Oct 10, 2006; 10:24:40

Unit cell

3146 reflections with 1.00°<theta<27.48° (resolution between 20.40A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p1

a (Angstrom) 7.7896 +/- 0.0003

b (Angstrom) 8.8065 +/- 0.0003

c (Angstrom) 10.7285 +/- 0.0004

alpha (°) 106.793 +/- 0.002

beta (°) 89.9767 +/- 0.0017

gamma (°) 90.061 +/- 0.002

Volume (A**3) 704.58 +/- 0.05
Mosaicity (°) 0.395 +/- 0.002

Symmetry used in scalepack	p1
a (Angstrom)	7.7896 +/- 0.0003
b (Angstrom)	8.8065 +/- 0.0003
c (Angstrom)	10.7285 +/- 0.0004
alpha (°)	106.793 +/- 0.002
beta (°)	89.9767 +/- 0.0017
gamma (°)	90.061 +/- 0.002
Volume (A**3)	704.58 +/- 0.05
Mosaicity (°)	0.395 +/- 0.002

Data collection

Summary

Total number of images collected	305
Total exposure time	101.1 minutes
Data collection exposure time	99.4 minutes
Data collection wall-clock time	123.8 minutes

Experimental Conditions

Wavelength	0.71073 A

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Detector distance	Used in scaling
cell determination	i01f	10	`10.0`° phi	1.000°	10 seconds	45.00 mm	No
data collection	s01f	181	`362.0`° phi	2.000°	20 seconds	31.00 mm	Yes
data collection	s02f	17	`34.0`° omega	2.000°	20 seconds	31.00 mm	Yes
data collection	s03f	17	`34.0`° omega	2.000°	20 seconds	31.00 mm	Yes
data collection	s04f	56	`112.0`° omega	2.000°	20 seconds	31.00 mm	Yes
data collection	s05f	24	`48.0`° omega	2.000°	20 seconds	31.00 mm	Yes

Scalepack Scaling

Deleted observations

Rejected	`60`
Overload or incomplete profile	`390`
Sigma cutoff	`19`

Final Data Set

Scale factor range	8.86-11.37
Number of 'full' reflections	`10472`
Number of 'partial' reflections	`4281`
Total number of integrated reflections	`14040`
Total number of unique reflections	`3243`
Data completeness	`99.2%`
Resolution range	20.40-0.77 A
Theta range	1.00°-27.48°
Average Intensity	`72.9`
Average Sigma(I)	`2.5`
Overall R-merge (linear)	`0.037`

Sadabs Results

Parameter refinement on 9588 reflections reduced R(int) from 0.5253 to 0.0523

Before rejection, 14040 reflections total and 2041 unique

After rejection, 8668 reflections total and 1732 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0616   0.927 - 1.160   0.926 - 1.125   1.371    5304    3578
    2   -7.8  0.0539   0.552 - 0.624   0.965 - 1.043   1.195     535     351
    3   -7.8  0.0572   0.884 - 1.022   0.961 - 1.127   1.295     497     336
    4   -7.8  0.0569   0.963 - 1.162   0.912 - 1.056   1.354    1585    1077
    5   -7.8  0.0584   0.552 - 0.608   0.912 - 1.070   1.261     747     496

Ratio of minimum to maximum apparent transmission: 0.809473

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp14 a10

Formula C8H12O5N1

Crystal Colour Colourless

Crystal Habit Rod

Crystal Size 0.58 x 0.18 x 0.16 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	wp14 a10
Formula	C8H12O5N1
Crystal Colour	Colourless
Crystal Habit	Rod
Crystal Size	0.58 x 0.18 x 0.16 (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/