Summary report for Directory: diska/06skc0062

Report generated Oct 12, 2006; 17:22:02

Unit cell

3319 reflections with 1.00°<theta<23.26° (resolution between 20.40A and 0.90A) were used for unit cell refinement

Symmetry used
in scalepack p2

a (Angstrom) 9.2008 +/- 0.0003

b (Angstrom) 23.6311 +/- 0.0010

c (Angstrom) 10.4061 +/- 0.0004

alpha (°) 90.000

beta (°) 95.173 +/- 0.003

gamma (°) 90.000

Volume (A**3) 2253.33 +/- 0.15
Mosaicity (°) 0.645 +/- 0.002

Symmetry used in scalepack	p2
a (Angstrom)	9.2008 +/- 0.0003
b (Angstrom)	23.6311 +/- 0.0010
c (Angstrom)	10.4061 +/- 0.0004
alpha (°)	90.000
beta (°)	95.173 +/- 0.003
gamma (°)	90.000
Volume (A**3)	2253.33 +/- 0.15
Mosaicity (°)	0.645 +/- 0.002

Data collection

Summary

Total number of images collected	362
Total exposure time	232.6 minutes
Data collection exposure time	230.0 minutes
Data collection wall-clock time	258.5 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°	15 seconds	45.00 mm	No
data collection	s01f	193	`250.9`° phi	1.300°	39 seconds	35.00 mm	Yes
data collection	s02f	26	`33.8`° omega	1.300°	39 seconds	35.00 mm	Yes
data collection	s03f	43	`55.9`° omega	1.300°	39 seconds	35.00 mm	Yes
data collection	s04f	90	`117.0`° omega	1.300°	39 seconds	35.00 mm	Yes

Scalepack Scaling

Deleted observations

Rejected	`121`
Zero sigma or profile test	`4`
Overload or incomplete profile	`704`
Sigma cutoff	`54`
High resolution limit	`16`

Final Data Set

Scale factor range	8.76-10.04
Number of 'full' reflections	`8061`
Number of 'partial' reflections	`15980`
Total number of integrated reflections	`22321`
Total number of unique reflections	`3340`
Data completeness	`100.0%`
Resolution range	20.40-0.90 A
Theta range	1.00°-23.26°
Average Intensity	`21.1`
Average Sigma(I)	`1.1`
Overall R-merge (linear)	`0.080`

Sadabs Results

Parameter refinement on 12242 reflections reduced R(int) from 0.0748 to 0.0467

Before rejection, 22980 reflections total and 3350 unique

After rejection, 22674 reflections total and 3348 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   11.8  0.0785   0.801 - 0.979   0.949 - 1.177   1.170   12648    7596
    2  -11.2  0.0775   0.478 - 0.508   0.961 - 1.025   1.151    1561     900
    3  -11.2  0.0713   1.570 - 1.682   0.935 - 1.108   1.174    2703    1563
    4  -11.2  0.0903   0.946 - 1.056   0.931 - 1.061   1.179    5762    3381

Ratio of minimum to maximum apparent transmission: 0.791076

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp14 h4

Formula c10H12O4N1

Crystal Colour Colourless

Crystal Habit Plate

Crystal Size 0.32 x 0.18 x 0.04 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	wp14 h4
Formula	c10H12O4N1
Crystal Colour	Colourless
Crystal Habit	Plate
Crystal Size	0.32 x 0.18 x 0.04 (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/