Summary report for Directory: diska/2008lsh018

Report generated Jul 05, 2008; 14:05:35

Unit cell

12717 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p222

a (Angstrom) 9.2804 +/- 0.0002

b (Angstrom) 9.3819 +/- 0.0002

c (Angstrom) 20.7436 +/- 0.0005

alpha (°) 90.000

beta (°) 90.000

gamma (°) 90.000

Volume (A**3) 1806.10 +/- 0.07
Mosaicity (°) 0.4810 +/- 0.0010

Symmetry used in scalepack	p222
a (Angstrom)	9.2804 +/- 0.0002
b (Angstrom)	9.3819 +/- 0.0002
c (Angstrom)	20.7436 +/- 0.0005
alpha (°)	90.000
beta (°)	90.000
gamma (°)	90.000
Volume (A**3)	1806.10 +/- 0.07
Mosaicity (°)	0.4810 +/- 0.0010

Data collection

Summary

Total number of images collected	192
Total exposure time	26.2 minutes
Data collection exposure time	25.5 minutes
Data collection wall-clock time	33.2 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	56	`89.6`° omega	1.600°	8 seconds	Yes
data collection	s02f	38	`60.8`° omega	1.600°	8 seconds	Yes
data collection	s03f	61	`97.6`° omega	1.600°	8 seconds	Yes
data collection	s04f	29	`46.4`° omega	1.600°	8 seconds	Yes
Phi/Chi	i01f - i08f	8			5 seconds

Scalepack Scaling

Deleted observations

Rejected	`4`
Overload or incomplete profile	`926`
Sigma cutoff	`262`
High resolution limit	`42`

Final Data Set

Scale factor	10.00
Number of 'full' reflections	`10276`
Number of 'partial' reflections	`7768`
Total number of integrated reflections	`16536`
Total number of unique reflections	`2361`
Data completeness	`99.3%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`366.0`
Average Sigma(I)	`6.4`
Overall R-merge (linear)	`0.131`

Sadabs Results

Parameter refinement on 12504 reflections reduced R(int) from 0.1040 to 0.0329

Before rejection, 16543 reflections total and 2376 unique

After rejection, 14951 reflections total and 2372 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1    4.4  0.0331   0.909 - 1.116   0.923 - 1.640   2.179    4696    3561
    2    8.8  0.0372   0.814 - 1.136   0.923 - 1.654   2.210    3059    2254
    3   -7.9  0.0309   0.689 - 0.963   0.923 - 1.582   2.087    4966    3692
    4   10.2  0.0349   0.819 - 0.898   0.929 - 1.457   2.172    2230    1647

Ratio of minimum to maximum apparent transmission: 0.557974

Metadata

Group Mike Hursthouse

Operator Susanne Huth

Sample Owner

Local Code PPA/Br

Formula C9 H10 Br1 N1 O1

Crystal Colour Colourless

Crystal Habit Cut Needle

Crystal Size 0.4 x 0.1 x 0.1 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Mike Hursthouse
Operator	Susanne Huth
Sample Owner
Local Code	PPA/Br
Formula	C9 H10 Br1 N1 O1
Crystal Colour	Colourless
Crystal Habit	Cut Needle
Crystal Size	0.4 x 0.1 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 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/