Summary report for Directory: home/diska/06skc0030

Report generated Jul 28, 2006; 07:33:17

Unit cell

4364 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) 5.6883 +/- 0.0006

b (Angstrom) 7.9063 +/- 0.0008

c (Angstrom) 24.124 +/- 0.003

alpha (°) 98.308 +/- 0.007

beta (°) 90.014 +/- 0.005

gamma (°) 89.973 +/- 0.006

Volume (A**3) 1073.5 +/- 0.2
Mosaicity (°) 2.195 +/- 0.004

Symmetry used in scalepack	p1
a (Angstrom)	5.6883 +/- 0.0006
b (Angstrom)	7.9063 +/- 0.0008
c (Angstrom)	24.124 +/- 0.003
alpha (°)	98.308 +/- 0.007
beta (°)	90.014 +/- 0.005
gamma (°)	89.973 +/- 0.006
Volume (A**3)	1073.5 +/- 0.2
Mosaicity (°)	2.195 +/- 0.004

Data collection

Summary

Total number of images collected	516
Total exposure time	279.6 minutes
Data collection exposure time	276.9 minutes
Data collection wall-clock time	5.3 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	31.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	279	`362.7`° phi	1.300°	32 seconds	Yes
data collection	s02f	25	`32.5`° omega	1.300°	32 seconds	Yes
data collection	s03f	84	`109.2`° omega	1.300°	32 seconds	Yes
data collection	s04f	36	`46.8`° omega	1.300°	32 seconds	Yes
data collection	s05f	84	`109.2`° omega	1.300°	32 seconds	Yes
Phi/Chi	i01f - i08f	8			20 seconds

Scalepack Scaling

Deleted observations

Rejected	`473`
Zero sigma or profile test	`40`
Overload or incomplete profile	`932`
Sigma cutoff	`76`
Low resolution limit	`10`
High resolution limit	`162`

Final Data Set

Scale factor range	3.06-13.68
Number of 'full' reflections	`0`
Number of 'partial' reflections	`21499`
Total number of integrated reflections	`18318`
Total number of unique reflections	`4736`
Data completeness	`95.6%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`20.8`
Average Sigma(I)	`1.8`
Overall R-merge (linear)	`0.126`

Sadabs Results

Parameter refinement on 11618 reflections reduced R(int) from 0.2098 to 0.0821

Before rejection, 23499 reflections total and 4957 unique

After rejection, 21749 reflections total and 4924 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.1030   0.756 - 1.007   0.886 - 1.726   1.363   12360    7402
    2   -7.8  0.1521   0.668 - 0.760   0.956 - 1.381   1.452     982     514
    3   -7.8  0.0974   0.826 - 1.258   0.886 - 1.304   1.321    3830    2265
    4   -7.8  0.2765   0.746 - 1.002   0.886 - 1.699   1.569    1304     402
    5   -7.8  0.2918   0.521 - 0.820   0.934 - 1.384   1.708    3273    1303

Ratio of minimum to maximum apparent transmission: 0.513216

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp7 g11

Formula C12H14O4N2S1

Crystal Colour Colourless

Crystal Habit Shard

Crystal Size 0.1 x 0.07 x 0.01 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	wp7 g11
Formula	C12H14O4N2S1
Crystal Colour	Colourless
Crystal Habit	Shard
Crystal Size	0.1 x 0.07 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/