Summary report for Directory: diska/2008lsh121

Report generated Nov 08, 2008; 19:42:59

Unit cell

4372 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack c2

a (Angstrom) 20.8029 +/- 0.0013

b (Angstrom) 4.7163 +/- 0.0003

c (Angstrom) 6.7095 +/- 0.0003

alpha (°) 90.000

beta (°) 105.889 +/- 0.004

gamma (°) 90.000

Volume (A**3) 633.14 +/- 0.06
Mosaicity (°) 0.757 +/- 0.004

Symmetry used in scalepack	c2
a (Angstrom)	20.8029 +/- 0.0013
b (Angstrom)	4.7163 +/- 0.0003
c (Angstrom)	6.7095 +/- 0.0003
alpha (°)	90.000
beta (°)	105.889 +/- 0.004
gamma (°)	90.000
Volume (A**3)	633.14 +/- 0.06
Mosaicity (°)	0.757 +/- 0.004

Data collection

Summary

Total number of images collected	209
Total exposure time	274.4 minutes
Data collection exposure time	269.1 minutes
Data collection wall-clock time	281.9 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	51	`102.0`° omega	2.000°	80 seconds	Yes
data collection	s02f	51	`102.0`° omega	2.000°	80 seconds	Yes
data collection	s03f	51	`102.0`° omega	2.000°	80 seconds	Yes
data collection	s04f	48	`96.0`° omega	2.000°	80 seconds	Yes
Phi/Chi	i01f - i08f	8			40 seconds

Scalepack Scaling

Deleted observations

Zero sigma or profile test	`1`
Overload or incomplete profile	`118`
Sigma cutoff	`38`
High resolution limit	`29`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`2032`
Number of 'partial' reflections	`2258`
Total number of integrated reflections	`4030`
Total number of unique reflections	`802`
Data completeness	`99.8%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`198.7`
Average Sigma(I)	`4.5`
Overall R-merge (linear)	`0.135`

Sadabs Results

Parameter refinement on 3554 reflections reduced R(int) from 0.1307 to 0.0423

Before rejection, 3984 reflections total and 811 unique

After rejection, 3631 reflections total and 808 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.1  0.0444   0.904 - 1.549   0.880 - 1.069   2.276     939     831
    2   10.2  0.0421   0.379 - 0.650   0.877 - 1.079   2.069     916     827
    3   10.2  0.0412   0.904 - 1.715   0.922 - 1.152   2.173     906     800
    4   10.2  0.0394   0.982 - 1.449   0.984 - 1.155   2.089     870     760

Ratio of minimum to maximum apparent transmission: 0.759853

Metadata

Group Mike Hursthouse

Operator Susanne Huth

Sample Owner

Local Code MMC/NO2

Formula C8 H8 N2 O3

Crystal Colour Colourless

Crystal Habit Needle

Crystal Size 0.44 x 0.02 x 0.01 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Susanne Huth
Sample Owner
Local Code	MMC/NO2
Formula	C8 H8 N2 O3
Crystal Colour	Colourless
Crystal Habit	Needle
Crystal Size	0.44 x 0.02 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 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    '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_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/