Summary report for Directory: diska/05src0137

Report generated Feb 01, 2005; 08:24:41

Unit cell

2588 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack p2

a (Angstrom) 6.5438 +/- 0.0004

b (Angstrom) 25.107 +/- 0.002

c (Angstrom) 8.4443 +/- 0.0006

alpha (°) 90.000

beta (°) 106.518 +/- 0.004

gamma (°) 90.000

Volume (A**3) 1330.11 +/- 0.17
Mosaicity (°) 0.632 +/- 0.003

Symmetry used in scalepack	p2
a (Angstrom)	6.5438 +/- 0.0004
b (Angstrom)	25.107 +/- 0.002
c (Angstrom)	8.4443 +/- 0.0006
alpha (°)	90.000
beta (°)	106.518 +/- 0.004
gamma (°)	90.000
Volume (A**3)	1330.11 +/- 0.17
Mosaicity (°)	0.632 +/- 0.003

Data collection

Summary

Total number of images collected	355
Total exposure time	13.1 hours
Data collection exposure time	13.0 hours
Data collection wall-clock time	13.6 hours

Experimental Conditions

Wavelength	0.71073 A
Crystal to detector distance	45.00 mm

Scans

Type	Name	# images	Total Rotation	Per frame Rotation	Exposure per frame	Used in scaling
data collection	s01f	176	`264.0`° phi	1.500°	135 seconds	Yes
data collection	s02f	22	`33.0`° omega	1.500°	135 seconds	Yes
data collection	s03f	90	`135.0`° omega	1.500°	135 seconds	Yes
data collection	s04f	59	`88.5`° omega	1.500°	135 seconds	Yes
Phi/Chi	i01f - i08f	8			50 seconds

Scalepack Scaling

Deleted observations

Rejected	`54`
Zero sigma or profile test	`47`
Overload or incomplete profile	`306`
Sigma cutoff	`26`
High resolution limit	`73`

Final Data Set

Scale factor range	9.34-10.35
Number of 'full' reflections	`6198`
Number of 'partial' reflections	`7374`
Total number of integrated reflections	`9230`
Total number of unique reflections	`3035`
Data completeness	`97.2%`
Resolution range	7.00-0.77 A
Theta range	2.91°-27.48°
Average Intensity	`38.1`
Average Sigma(I)	`2.1`
Overall R-merge (linear)	`0.047`

Sadabs Results

Parameter refinement on 8117 reflections reduced R(int) from 0.1245 to 0.0369

Before rejection, 14831 reflections total and 3154 unique

After rejection, 14599 reflections total and 3151 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   18.9  0.0496   0.763 - 0.942   0.949 - 1.137   1.230    7406    4530
    2  -18.3  0.0446   1.105 - 1.237   0.972 - 1.204   1.238     863     514
    3  -18.3  0.0447   0.831 - 0.994   0.955 - 1.109   1.202    3852    2381
    4  -18.3  0.0439   1.225 - 1.357   0.949 - 1.096   1.180    2478    1471

Ratio of minimum to maximum apparent transmission: 0.788189

Metadata

Group Service

Operator Peter Horton

Sample Owner Dr. A. K. Croft

Local Code A 692

Formula C17 H15 Br1

Crystal Colour Colourless

Crystal Habit Cut Shard

Crystal Size 0.22 x 0.14 x 0.03 (mm3)

Temperature 120(K)

Generator 50 (kV) 85 (mA)

Primary Solvent

Other Solvents

Group	Service
Operator	Peter Horton
Sample Owner	Dr. A. K. Croft
Local Code	A 692
Formula	C17 H15 Br1
Crystal Colour	Colourless
Crystal Habit	Cut Shard
Crystal Size	0.22 x 0.14 x 0.03 (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/