Summary report for Directory: diska/06skc0036

Report generated Aug 24, 2006; 10:15:31

Unit cell

1052 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) 9.6872 +/- 0.0005

b (Angstrom) 6.5461 +/- 0.0003

c (Angstrom) 10.8209 +/- 0.0005

alpha (°) 90.000

beta (°) 102.698 +/- 0.003

gamma (°) 90.000

Volume (A**3) 669.41 +/- 0.06
Mosaicity (°) 0.587 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	9.6872 +/- 0.0005
b (Angstrom)	6.5461 +/- 0.0003
c (Angstrom)	10.8209 +/- 0.0005
alpha (°)	90.000
beta (°)	102.698 +/- 0.003
gamma (°)	90.000
Volume (A**3)	669.41 +/- 0.06
Mosaicity (°)	0.587 +/- 0.003

Data collection

Summary

Total number of images collected	214
Total exposure time	140.1 minutes
Data collection exposure time	136.7 minutes
Data collection wall-clock time	153.1 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°	20 seconds	45.00 mm	No
data collection	s01f	99	`198.0`° phi	2.000°	40 seconds	31.00 mm	Yes
data collection	s02f	51	`102.0`° omega	2.000°	40 seconds	31.00 mm	Yes
data collection	s03f	54	`108.0`° omega	2.000°	40 seconds	31.00 mm	Yes

Scalepack Scaling

Deleted observations

Rejected	`32`
Overload or incomplete profile	`150`
Sigma cutoff	`8`
High resolution limit	`14`

Final Data Set

Scale factor range	9.72-10.63
Number of 'full' reflections	`4351`
Number of 'partial' reflections	`3153`
Total number of integrated reflections	`7232`
Total number of unique reflections	`1056`
Data completeness	`99.7%`
Resolution range	20.40-0.90 A
Theta range	1.00°-23.26°
Average Intensity	`92.1`
Average Sigma(I)	`1.9`
Overall R-merge (linear)	`0.032`

Sadabs Results

Parameter refinement on 5377 reflections reduced R(int) from 0.0580 to 0.0288

Before rejection, 7174 reflections total and 1062 unique

After rejection, 7124 reflections total and 1061 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    8.3  0.0302   1.095 - 1.229   0.958 - 1.126   1.188    3512    2744
    2   -7.8  0.0336   0.628 - 0.670   0.934 - 1.022   1.121    1746    1358
    3   -7.8  0.0338   1.011 - 1.142   0.956 - 1.069   1.136    1866    1480

Ratio of minimum to maximum apparent transmission: 0.829421

Metadata

Group Mike Hursthouse

Operator Sam Callear

Sample Owner

Local Code wp8 a7

Formula C6H10O5N1

Crystal Colour Colourless

Crystal Habit Block

Crystal Size 0.24 x 0.18 x 0.1 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Sam Callear
Sample Owner
Local Code	wp8 a7
Formula	C6H10O5N1
Crystal Colour	Colourless
Crystal Habit	Block
Crystal Size	0.24 x 0.18 x 0.1 (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/